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#$Date: 2024-10-06 08:00:21 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/36/7133686.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133686
loop_
_publ_author_name
'Kennedy, Dominic B.'
'Evans, Matthew J.'
'Jones, Dafydd D. L.'
'Parr, Joseph M.'
'Hill, Michael S.'
'Jones, Cameron'
_publ_section_title
;
 A series of neutral alkaline earth metal hydride complexes supported by a
 bulky, unsymmetrical β-diketiminate ligand,
 [{(<sup>Dip/TCHP</sup>Nacnac)M(μ-H)}₂] (M = Mg, Ca, Sr
 or Ba).
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10894
_journal_page_last               10897
_journal_paper_doi               10.1039/d4cc04286g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C100 H138 Ca2 N4 O0.4'
_chemical_formula_weight         1482.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                106.3540(10)
_cell_angle_beta                 102.1740(10)
_cell_angle_gamma                113.558(2)
_cell_formula_units_Z            1
_cell_length_a                   12.5680(2)
_cell_length_b                   14.4876(2)
_cell_length_c                   14.5826(2)
_cell_measurement_reflns_used    19780
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      79.1300
_cell_measurement_theta_min      3.6160
_cell_volume                     2171.82(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'w\ scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27837
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.796
_diffrn_reflns_theta_min         6.392
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       plate
_exptl_crystal_F_000             809
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.807
_exptl_transmission_factor_min   0.725
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0680P)²+0.5892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8536
_reflns_number_total             8957
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc04286g2.cif
_cod_data_source_block           cj1697
_cod_depositor_comments
'Adding full bibliography for 7133684--7133690.cif.'
_cod_original_cell_volume        2171.82(6)
_cod_original_formula_sum        'C100 H138 Ca2 N4 O0.40'
_cod_database_code               7133686
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.807
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.61262(2) 0.11360(2) 0.61102(2) 0.02522(9) Uani 1 1 d . . . . .
N1 N 0.75393(9) 0.28565(9) 0.75702(8) 0.0217(2) Uani 1 1 d . . . . .
C1 C 0.85551(11) 0.27633(9) 0.81110(9) 0.0215(2) Uani 1 1 d . . . . .
N2 N 0.52398(9) 0.23194(9) 0.60110(8) 0.0235(2) Uani 1 1 d . . . . .
C2 C 0.84870(11) 0.24061(10) 0.89125(9) 0.0229(2) Uani 1 1 d . . . . .
C3 C 0.74356(12) 0.23089(10) 0.93086(10) 0.0243(2) Uani 1 1 d . . . . .
H3 H 0.718205 0.284455 0.917337 0.029 Uiso 1 1 calc R U . . .
C4 C 0.62695(12) 0.11649(11) 0.87467(10) 0.0281(3) Uani 1 1 d . . . . .
H4A H 0.599728 0.096807 0.799777 0.034 Uiso 1 1 calc R U . . .
H4B H 0.647697 0.061024 0.887467 0.034 Uiso 1 1 calc R U . . .
C5 C 0.52056(13) 0.11374(12) 0.91050(11) 0.0332(3) Uani 1 1 d . . . . .
H5A H 0.448099 0.038215 0.875157 0.040 Uiso 1 1 calc R U . . .
H5B H 0.494439 0.164164 0.891946 0.040 Uiso 1 1 calc R U . . .
C6 C 0.56082(14) 0.14837(12) 1.02665(11) 0.0349(3) Uani 1 1 d . . . . .
H6A H 0.492351 0.150903 1.048673 0.042 Uiso 1 1 calc R U . . .
H6B H 0.577388 0.092974 1.044230 0.042 Uiso 1 1 calc R U . . .
C7 C 0.67769(14) 0.26105(12) 1.08384(11) 0.0330(3) Uani 1 1 d . . . . .
H7A H 0.704733 0.279255 1.158467 0.040 Uiso 1 1 calc R U . . .
H7B H 0.658504 0.317830 1.072532 0.040 Uiso 1 1 calc R U . . .
C8 C 0.78316(13) 0.26255(12) 1.04704(10) 0.0300(3) Uani 1 1 d . . . . .
H8A H 0.807033 0.210111 1.063580 0.036 Uiso 1 1 calc R U . . .
H8B H 0.857005 0.337235 1.083645 0.036 Uiso 1 1 calc R U . . .
C9 C 0.94165(12) 0.21906(10) 0.93466(10) 0.0242(2) Uani 1 1 d . . . . .
H9 H 0.936753 0.194039 0.988044 0.029 Uiso 1 1 calc R U . . .
C10 C 1.04146(12) 0.23325(10) 0.90180(10) 0.0241(2) Uani 1 1 d . . . . .
C11 C 1.14068(12) 0.20718(11) 0.94709(10) 0.0261(3) Uani 1 1 d . . . . .
H11 H 1.199990 0.221840 0.910064 0.031 Uiso 1 1 calc R U . . .
C12 C 1.08576(15) 0.08544(13) 0.92826(14) 0.0414(4) Uani 1 1 d . . . . .
H12A H 1.043323 0.039384 0.853444 0.050 Uiso 1 1 calc R U . . .
H12B H 1.022719 0.066547 0.960507 0.050 Uiso 1 1 calc R U . . .
C13 C 1.18713(17) 0.05980(15) 0.97250(16) 0.0467(4) Uani 1 1 d . . . . .
H13A H 1.147956 -0.018445 0.962627 0.056 Uiso 1 1 calc R U . . .
H13B H 1.244960 0.070793 0.934854 0.056 Uiso 1 1 calc R U . . .
C14 C 1.25932(17) 0.13214(19) 1.08468(15) 0.0506(5) Uani 1 1 d . . . . .
H14A H 1.326659 0.116076 1.109933 0.061 Uiso 1 1 calc R U . . .
H14B H 1.203206 0.115656 1.123297 0.061 Uiso 1 1 calc R U . . .
C15 C 1.31629(17) 0.25412(17) 1.10438(13) 0.0489(4) Uani 1 1 d . . . . .
H15A H 1.379782 0.272562 1.072504 0.059 Uiso 1 1 calc R U . . .
H15B H 1.358526 0.299636 1.179298 0.059 Uiso 1 1 calc R U . . .
C16 C 1.21629(16) 0.28147(15) 1.06015(12) 0.0420(4) Uani 1 1 d . . . . .
H16A H 1.159614 0.272995 1.098877 0.050 Uiso 1 1 calc R U . . .
H16B H 1.257001 0.359298 1.068862 0.050 Uiso 1 1 calc R U . . .
C17 C 1.04903(11) 0.27431(10) 0.82640(10) 0.0232(2) Uani 1 1 d . . . . .
H17 H 1.118100 0.286863 0.805092 0.028 Uiso 1 1 calc R U . . .
C18 C 0.95916(11) 0.29778(10) 0.78085(9) 0.0221(2) Uani 1 1 d . . . . .
C19 C 0.97356(12) 0.34901(10) 0.70337(10) 0.0238(2) Uani 1 1 d . . . . .
H19 H 0.924760 0.389215 0.706208 0.029 Uiso 1 1 calc R U . . .
C20 C 1.10906(13) 0.43409(11) 0.72888(11) 0.0305(3) Uani 1 1 d . . . . .
H20A H 1.142923 0.490809 0.799699 0.037 Uiso 1 1 calc R U . . .
H20B H 1.160326 0.397059 0.725824 0.037 Uiso 1 1 calc R U . . .
C21 C 1.11778(14) 0.48977(12) 0.65363(11) 0.0342(3) Uani 1 1 d . . . . .
H21A H 1.073304 0.532825 0.661537 0.041 Uiso 1 1 calc R U . . .
H21B H 1.206444 0.541565 0.670030 0.041 Uiso 1 1 calc R U . . .
C22 C 1.06131(14) 0.40527(13) 0.54307(11) 0.0343(3) Uani 1 1 d . . . . .
H22A H 1.112176 0.368593 0.532932 0.041 Uiso 1 1 calc R U . . .
H22B H 1.062671 0.443182 0.496111 0.041 Uiso 1 1 calc R U . . .
C23 C 0.92736(14) 0.31876(13) 0.51683(11) 0.0364(3) Uani 1 1 d . . . . .
H23A H 0.894924 0.262100 0.446206 0.044 Uiso 1 1 calc R U . . .
H23B H 0.874363 0.354141 0.519068 0.044 Uiso 1 1 calc R U . . .
C24 C 0.92022(13) 0.26363(11) 0.59242(10) 0.0293(3) Uani 1 1 d . . . . .
H24A H 0.967656 0.223158 0.586069 0.035 Uiso 1 1 calc R U . . .
H24B H 0.832119 0.209633 0.575093 0.035 Uiso 1 1 calc R U . . .
C25 C 0.75549(11) 0.38152(10) 0.79314(9) 0.0227(2) Uani 1 1 d . . . . .
C26 C 0.86428(12) 0.47693(11) 0.88791(10) 0.0279(3) Uani 1 1 d . . . . .
H26A H 0.863874 0.458922 0.947815 0.042 Uiso 1 1 calc R U . . .
H26B H 0.856366 0.543480 0.899346 0.042 Uiso 1 1 calc R U . . .
H26C H 0.942807 0.489959 0.877719 0.042 Uiso 1 1 calc R U . . .
C27 C 0.66154(12) 0.40217(10) 0.74965(10) 0.0252(3) Uani 1 1 d . . . . .
H27 H 0.672937 0.473385 0.785086 0.030 Uiso 1 1 calc R U . . .
C28 C 0.55257(12) 0.33243(11) 0.66088(10) 0.0242(2) Uani 1 1 d . . . . .
C29 C 0.46823(13) 0.38108(11) 0.63859(11) 0.0302(3) Uani 1 1 d . . . . .
H29A H 0.407438 0.336637 0.567971 0.045 Uiso 1 1 calc R U . . .
H29B H 0.518744 0.456928 0.646873 0.045 Uiso 1 1 calc R U . . .
H29C H 0.424099 0.381064 0.686552 0.045 Uiso 1 1 calc R U . . .
C30 C 0.41551(11) 0.16468(10) 0.50956(10) 0.0232(2) Uani 1 1 d . . . . .
C31 C 0.29843(12) 0.10037(11) 0.51269(10) 0.0248(3) Uani 1 1 d . . . . .
C32 C 0.27453(13) 0.11794(12) 0.61247(11) 0.0305(3) Uani 1 1 d . . . . .
H32 H 0.354562 0.177256 0.669891 0.037 Uiso 1 1 calc R U . . .
C33 C 0.23101(16) 0.01423(14) 0.63489(13) 0.0389(3) Uani 1 1 d . . . . .
H33A H 0.148503 -0.042819 0.583266 0.058 Uiso 1 1 calc R U . . .
H33B H 0.226126 0.032450 0.703349 0.058 Uiso 1 1 calc R U . . .
H33C H 0.290628 -0.013112 0.632371 0.058 Uiso 1 1 calc R U . . .
C34 C 0.17795(15) 0.15744(14) 0.61074(13) 0.0401(4) Uani 1 1 d . . . . .
H34A H 0.207356 0.225143 0.598937 0.060 Uiso 1 1 calc R U . . .
H34B H 0.166533 0.172205 0.676773 0.060 Uiso 1 1 calc R U . . .
H34C H 0.098246 0.100216 0.555405 0.060 Uiso 1 1 calc R U . . .
C35 C 0.20159(12) 0.01878(11) 0.42063(10) 0.0261(3) Uani 1 1 d . . . . .
H35 H 0.122711 -0.025804 0.421868 0.031 Uiso 1 1 calc R U . . .
C36 C 0.21807(12) 0.00143(11) 0.32741(10) 0.0270(3) Uani 1 1 d . . . . .
H36 H 0.152024 -0.056247 0.265810 0.032 Uiso 1 1 calc R U . . .
C37 C 0.33166(12) 0.06884(11) 0.32464(10) 0.0269(3) Uani 1 1 d . . . . .
H37 H 0.341507 0.058658 0.260321 0.032 Uiso 1 1 calc R U . . .
C38 C 0.43186(12) 0.15142(10) 0.41460(10) 0.0246(3) Uani 1 1 d . . . . .
C39 C 0.55485(12) 0.22817(11) 0.41112(10) 0.0288(3) Uani 1 1 d . . . . .
H39 H 0.623172 0.245389 0.473568 0.035 Uiso 1 1 calc R U . . .
C40 C 0.56004(17) 0.33725(13) 0.41741(14) 0.0420(4) Uani 1 1 d . . . . .
H40A H 0.494655 0.323434 0.356733 0.063 Uiso 1 1 calc R U . . .
H40B H 0.641883 0.387665 0.419997 0.063 Uiso 1 1 calc R U . . .
H40C H 0.546920 0.370486 0.479524 0.063 Uiso 1 1 calc R U . . .
C41 C 0.58216(14) 0.17858(13) 0.31724(11) 0.0351(3) Uani 1 1 d . . . . .
H41A H 0.575347 0.107353 0.312033 0.053 Uiso 1 1 calc R U . . .
H41B H 0.666786 0.228786 0.324708 0.053 Uiso 1 1 calc R U . . .
H41C H 0.521798 0.167890 0.254974 0.053 Uiso 1 1 calc R U . . .
C42 C 0.9716(3) 0.6905(2) 0.72689(14) 0.0715(8) Uani 1 1 d . . . . .
H42 H 1.026363 0.668906 0.758409 0.086 Uiso 1 1 calc R U . . .
C43 C 1.0192(2) 0.7939(2) 0.72576(16) 0.0623(6) Uani 1 1 d . . . . .
H43 H 1.106587 0.843133 0.755746 0.075 Uiso 1 1 calc R U . . .
C44 C 0.93975(17) 0.82515(14) 0.68117(14) 0.0449(4) Uani 1 1 d . . . . .
H44 H 0.972246 0.896239 0.680159 0.054 Uiso 1 1 calc R U . . .
C45 C 0.81343(16) 0.75413(14) 0.63798(13) 0.0422(4) Uani 1 1 d . . . . .
H45 H 0.758883 0.776730 0.607952 0.051 Uiso 1 1 calc R U . . .
C46 C 0.7654(2) 0.65091(16) 0.63782(17) 0.0543(5) Uani 1 1 d . . . . .
H46 H 0.677906 0.601921 0.607239 0.065 Uiso 1 1 calc R U . . .
C47 C 0.8445(3) 0.61826(19) 0.68226(18) 0.0665(7) Uani 1 1 d . . . . .
H47 H 0.811764 0.546687 0.682177 0.080 Uiso 1 1 calc R U . . .
C48 C 0.52340(17) 0.42543(16) 0.93676(15) 0.0482(4) Uani 1 1 d . . . . .
H48 H 0.539436 0.374212 0.893229 0.058 Uiso 1 1 calc R U . . .
C49 C 0.61298(16) 0.50268(17) 1.03185(15) 0.0491(4) Uani 1 1 d . . . . .
H49 H 0.690856 0.504628 1.053977 0.059 Uiso 1 1 calc R U . . .
C50 C 0.58952(16) 0.57707(16) 1.09480(14) 0.0490(4) Uani 1 1 d . . . . .
H50 H 0.651434 0.630260 1.160191 0.059 Uiso 1 1 calc R U . . .
O1 O 0.3872(5) -0.0514(4) 0.5909(4) 0.0346(11) Uani 0.2 1 d D . P A 1
H H 0.4329(18) -0.0336(16) 0.5430(15) 0.023(5) Uiso 0.8 1 d . . P B 2
H1 H 0.3077(19) -0.056(4) 0.571(6) 0.028 Uiso 0.2 1 d D U P C 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ca1 N2 74.90(4) . . ?
N1 Ca1 O1 127.73(11) . . ?
N2 Ca1 O1 91.14(11) . . ?
N1 Ca1 O1 127.81(11) . 2_656 ?
N2 Ca1 O1 97.02(10) . 2_656 ?
O1 Ca1 O1 103.46(15) . 2_656 ?
N1 Ca1 C30 101.74(4) . . ?
N2 Ca1 C30 26.85(3) . . ?
O1 Ca1 C30 75.11(11) . . ?
O1 Ca1 C30 80.09(10) 2_656 . ?
N1 Ca1 C1 25.37(3) . . ?
N2 Ca1 C1 100.26(3) . . ?
O1 Ca1 C1 128.58(11) . . ?
O1 Ca1 C1 124.17(11) 2_656 . ?
C30 Ca1 C1 127.09(3) . . ?
N1 Ca1 Ca1 171.44(3) . 2_656 ?
N2 Ca1 Ca1 96.64(3) . 2_656 ?
O1 Ca1 Ca1 52.49(11) . 2_656 ?
O1 Ca1 Ca1 50.97(11) 2_656 2_656 ?
C30 Ca1 Ca1 69.78(2) . 2_656 ?
C1 Ca1 Ca1 162.99(3) . 2_656 ?
N1 Ca1 H 146.4(5) . . ?
N2 Ca1 H 93.4(5) . . ?
C30 Ca1 H 71.1(5) . . ?
C1 Ca1 H 145.9(5) . . ?
Ca1 Ca1 H 33.4(5) 2_656 . ?
N1 Ca1 H 143.0(6) . 2_656 ?
N2 Ca1 H 97.7(6) . 2_656 ?
O1 Ca1 H 87.9(6) . 2_656 ?
O1 Ca1 H 15.5(6) 2_656 2_656 ?
C30 Ca1 H 75.8(6) . 2_656 ?
C1 Ca1 H 138.4(6) . 2_656 ?
Ca1 Ca1 H 35.4(6) 2_656 2_656 ?
H Ca1 H 68.8(9) . 2_656 ?
C25 N1 C1 117.85(10) . . ?
C25 N1 Ca1 133.60(8) . . ?
C1 N1 Ca1 108.54(7) . . ?
C18 C1 C2 120.34(11) . . ?
C18 C1 N1 119.83(11) . . ?
C2 C1 N1 119.77(11) . . ?
C18 C1 Ca1 107.44(8) . . ?
C2 C1 Ca1 110.89(8) . . ?
N1 C1 Ca1 46.09(5) . . ?
C28 N2 C30 122.16(11) . . ?
C28 N2 Ca1 134.42(9) . . ?
C30 N2 Ca1 103.33(7) . . ?
C9 C2 C1 118.85(11) . . ?
C9 C2 C3 121.85(11) . . ?
C1 C2 C3 119.26(11) . . ?
C2 C3 C8 113.48(11) . . ?
C2 C3 C4 113.36(11) . . ?
C8 C3 C4 109.19(11) . . ?
C2 C3 H3 106.8 . . ?
C8 C3 H3 106.8 . . ?
C4 C3 H3 106.8 . . ?
C5 C4 C3 111.40(11) . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C4 C5 C6 110.91(12) . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 111.17(12) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 110.98(12) . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 C3 111.16(11) . . ?
C7 C8 H8A 109.4 . . ?
C3 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
C3 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C2 121.87(12) . . ?
C10 C9 H9 119.1 . . ?
C2 C9 H9 119.1 . . ?
C17 C10 C9 117.81(12) . . ?
C17 C10 C11 120.29(11) . . ?
C9 C10 C11 121.89(12) . . ?
C16 C11 C10 112.57(11) . . ?
C16 C11 C12 111.31(13) . . ?
C10 C11 C12 111.92(11) . . ?
C16 C11 H11 106.9 . . ?
C10 C11 H11 106.9 . . ?
C12 C11 H11 106.9 . . ?
C11 C12 C13 111.39(13) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C12 111.50(15) . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 C15 111.26(14) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 111.31(15) . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C11 C16 C15 111.78(13) . . ?
C11 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
C11 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
C10 C17 C18 122.63(12) . . ?
C10 C17 H17 118.7 . . ?
C18 C17 H17 118.7 . . ?
C17 C18 C1 118.27(11) . . ?
C17 C18 C19 121.58(11) . . ?
C1 C18 C19 120.10(11) . . ?
C18 C19 C24 113.35(10) . . ?
C18 C19 C20 113.08(11) . . ?
C24 C19 C20 109.14(11) . . ?
C18 C19 H19 107.0 . . ?
C24 C19 H19 107.0 . . ?
C20 C19 H19 107.0 . . ?
C21 C20 C19 111.25(12) . . ?
C21 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C22 C21 C20 111.33(12) . . ?
C22 C21 H21A 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C21 C22 C23 111.15(12) . . ?
C21 C22 H22A 109.4 . . ?
C23 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 C24 110.98(12) . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 C19 111.21(11) . . ?
C23 C24 H24A 109.4 . . ?
C19 C24 H24A 109.4 . . ?
C23 C24 H24B 109.4 . . ?
C19 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N1 C25 C27 124.29(11) . . ?
N1 C25 C26 119.74(11) . . ?
C27 C25 C26 115.97(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 C28 129.22(12) . . ?
C25 C27 H27 115.4 . . ?
C28 C27 H27 115.4 . . ?
N2 C28 C27 123.32(12) . . ?
N2 C28 C29 121.81(11) . . ?
C27 C28 C29 114.87(11) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C38 120.60(11) . . ?
C31 C30 N2 120.94(11) . . ?
C38 C30 N2 117.79(11) . . ?
C31 C30 Ca1 111.23(8) . . ?
C38 C30 Ca1 99.24(8) . . ?
N2 C30 Ca1 49.81(6) . . ?
C35 C31 C30 118.52(12) . . ?
C35 C31 C32 119.30(12) . . ?
C30 C31 C32 122.17(11) . . ?
C31 C32 C34 110.18(12) . . ?
C31 C32 C33 113.04(12) . . ?
C34 C32 C33 109.61(12) . . ?
C31 C32 H32 107.9 . . ?
C34 C32 H32 107.9 . . ?
C33 C32 H32 107.9 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C31 121.39(12) . . ?
C36 C35 H35 119.3 . . ?
C31 C35 H35 119.3 . . ?
C35 C36 C37 119.58(12) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C36 C37 C38 121.31(12) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 H37 119.3 . . ?
C37 C38 C30 118.44(12) . . ?
C37 C38 C39 121.23(12) . . ?
C30 C38 C39 120.30(11) . . ?
C38 C39 C40 110.41(12) . . ?
C38 C39 C41 114.31(11) . . ?
C40 C39 C41 109.85(12) . . ?
C38 C39 H39 107.3 . . ?
C40 C39 H39 107.3 . . ?
C41 C39 H39 107.3 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C47 120.19(19) . . ?
C43 C42 H42 119.9 . . ?
C47 C42 H42 119.9 . . ?
C44 C43 C42 119.7(2) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C43 C44 C45 120.21(19) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C46 C45 C44 120.53(17) . . ?
C46 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C45 C46 C47 119.8(2) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 H46 120.1 . . ?
C46 C47 C42 119.53(19) . . ?
C46 C47 H47 120.2 . . ?
C42 C47 H47 120.2 . . ?
C50 C48 C49 119.68(18) 2_667 . ?
C50 C48 H48 120.2 2_667 . ?
C49 C48 H48 120.2 . . ?
C50 C49 C48 120.03(17) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C48 C50 C49 120.28(17) 2_667 . ?
C48 C50 H50 119.9 2_667 . ?
C49 C50 H50 119.9 . . ?
Ca1 O1 Ca1 76.54(15) . 2_656 ?
Ca1 O1 H1 128(3) . . ?
Ca1 O1 H1 94(5) 2_656 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 N1 2.4038(10) . ?
Ca1 N2 2.4083(11) . ?
Ca1 O1 2.769(6) . ?
Ca1 O1 2.827(6) 2_656 ?
Ca1 C30 3.0676(12) . ?
Ca1 C1 3.1633(12) . ?
Ca1 Ca1 3.4664(5) 2_656 ?
Ca1 H 2.16(2) . ?
Ca1 H 2.04(2) 2_656 ?
N1 C25 1.3299(17) . ?
N1 C1 1.4294(15) . ?
C1 C18 1.4086(17) . ?
C1 C2 1.4102(18) . ?
N2 C28 1.3205(17) . ?
N2 C30 1.4241(15) . ?
C2 C9 1.3979(18) . ?
C2 C3 1.5227(17) . ?
C3 C8 1.5339(18) . ?
C3 C4 1.5341(18) . ?
C3 H3 1.0000 . ?
C4 C5 1.5252(19) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.528(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.523(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.5262(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.3958(19) . ?
C9 H9 0.9500 . ?
C10 C17 1.3925(18) . ?
C10 C11 1.5177(17) . ?
C11 C16 1.517(2) . ?
C11 C12 1.529(2) . ?
C11 H11 1.0000 . ?
C12 C13 1.531(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.499(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.528(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.534(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.3965(18) . ?
C17 H17 0.9500 . ?
C18 C19 1.5203(17) . ?
C19 C24 1.5329(18) . ?
C19 C20 1.5344(18) . ?
C19 H19 1.0000 . ?
C20 C21 1.5314(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.521(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.524(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.530(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C27 1.3998(18) . ?
C25 C26 1.5187(17) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.4078(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.5188(18) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.4114(18) . ?
C30 C38 1.4136(18) . ?
C31 C35 1.3957(18) . ?
C31 C32 1.5195(18) . ?
C32 C34 1.534(2) . ?
C32 C33 1.536(2) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.3864(19) . ?
C35 H35 0.9500 . ?
C36 C37 1.3875(19) . ?
C36 H36 0.9500 . ?
C37 C38 1.3976(18) . ?
C37 H37 0.9500 . ?
C38 C39 1.5229(18) . ?
C39 C40 1.531(2) . ?
C39 C41 1.5327(19) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.379(4) . ?
C42 C47 1.384(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.371(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.372(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.370(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.382(3) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 C50 1.379(3) 2_667 ?
C48 C49 1.380(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.379(3) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
O1 H1 0.9501(10) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C25 N1 C1 C18 -93.27(14) . . . . ?
Ca1 N1 C1 C18 85.85(11) . . . . ?
C25 N1 C1 C2 89.75(14) . . . . ?
Ca1 N1 C1 C2 -91.12(11) . . . . ?
C25 N1 C1 Ca1 -179.13(14) . . . . ?
C18 C1 C2 C9 -4.72(17) . . . . ?
N1 C1 C2 C9 172.24(11) . . . . ?
Ca1 C1 C2 C9 121.79(10) . . . . ?
C18 C1 C2 C3 172.92(11) . . . . ?
N1 C1 C2 C3 -10.12(17) . . . . ?
Ca1 C1 C2 C3 -60.57(12) . . . . ?
C9 C2 C3 C8 33.50(17) . . . . ?
C1 C2 C3 C8 -144.07(12) . . . . ?
C9 C2 C3 C4 -91.81(14) . . . . ?
C1 C2 C3 C4 90.62(14) . . . . ?
C2 C3 C4 C5 -175.05(11) . . . . ?
C8 C3 C4 C5 57.36(15) . . . . ?
C3 C4 C5 C6 -56.67(16) . . . . ?
C4 C5 C6 C7 55.20(17) . . . . ?
C5 C6 C7 C8 -55.50(17) . . . . ?
C6 C7 C8 C3 57.19(16) . . . . ?
C2 C3 C8 C7 175.00(11) . . . . ?
C4 C3 C8 C7 -57.49(15) . . . . ?
C1 C2 C9 C10 0.83(18) . . . . ?
C3 C2 C9 C10 -176.75(11) . . . . ?
C2 C9 C10 C17 2.58(18) . . . . ?
C2 C9 C10 C11 -178.47(11) . . . . ?
C17 C10 C11 C16 114.40(15) . . . . ?
C9 C10 C11 C16 -64.53(17) . . . . ?
C17 C10 C11 C12 -119.34(14) . . . . ?
C9 C10 C11 C12 61.73(17) . . . . ?
C16 C11 C12 C13 -54.14(19) . . . . ?
C10 C11 C12 C13 178.92(14) . . . . ?
C11 C12 C13 C14 55.7(2) . . . . ?
C12 C13 C14 C15 -56.18(19) . . . . ?
C13 C14 C15 C16 55.3(2) . . . . ?
C10 C11 C16 C15 -179.80(14) . . . . ?
C12 C11 C16 C15 53.61(19) . . . . ?
C14 C15 C16 C11 -54.1(2) . . . . ?
C9 C10 C17 C18 -2.22(18) . . . . ?
C11 C10 C17 C18 178.81(11) . . . . ?
C10 C17 C18 C1 -1.55(18) . . . . ?
C10 C17 C18 C19 176.26(11) . . . . ?
C2 C1 C18 C17 5.05(17) . . . . ?
N1 C1 C18 C17 -171.90(11) . . . . ?
Ca1 C1 C18 C17 -123.03(10) . . . . ?
C2 C1 C18 C19 -172.79(11) . . . . ?
N1 C1 C18 C19 10.25(17) . . . . ?
Ca1 C1 C18 C19 59.12(12) . . . . ?
C17 C18 C19 C24 88.08(14) . . . . ?
C1 C18 C19 C24 -94.14(14) . . . . ?
C17 C18 C19 C20 -36.83(16) . . . . ?
C1 C18 C19 C20 140.95(12) . . . . ?
C18 C19 C20 C21 -175.69(11) . . . . ?
C24 C19 C20 C21 57.15(15) . . . . ?
C19 C20 C21 C22 -56.45(16) . . . . ?
C20 C21 C22 C23 54.92(17) . . . . ?
C21 C22 C23 C24 -55.26(17) . . . . ?
C22 C23 C24 C19 57.26(16) . . . . ?
C18 C19 C24 C23 175.33(11) . . . . ?
C20 C19 C24 C23 -57.66(15) . . . . ?
C1 N1 C25 C27 -178.68(12) . . . . ?
Ca1 N1 C25 C27 2.5(2) . . . . ?
C1 N1 C25 C26 1.04(17) . . . . ?
Ca1 N1 C25 C26 -177.82(9) . . . . ?
N1 C25 C27 C28 -2.6(2) . . . . ?
C26 C25 C27 C28 177.68(13) . . . . ?
C30 N2 C28 C27 -177.53(12) . . . . ?
Ca1 N2 C28 C27 6.4(2) . . . . ?
C30 N2 C28 C29 2.95(19) . . . . ?
Ca1 N2 C28 C29 -173.08(9) . . . . ?
C25 C27 C28 N2 -1.9(2) . . . . ?
C25 C27 C28 C29 177.69(13) . . . . ?
C28 N2 C30 C31 -84.42(16) . . . . ?
Ca1 N2 C30 C31 92.66(12) . . . . ?
C28 N2 C30 C38 104.91(14) . . . . ?
Ca1 N2 C30 C38 -78.01(11) . . . . ?
C28 N2 C30 Ca1 -177.09(14) . . . . ?
C38 C30 C31 C35 4.01(19) . . . . ?
N2 C30 C31 C35 -166.40(12) . . . . ?
Ca1 C30 C31 C35 -111.45(11) . . . . ?
C38 C30 C31 C32 -175.40(12) . . . . ?
N2 C30 C31 C32 14.20(19) . . . . ?
Ca1 C30 C31 C32 69.15(14) . . . . ?
C35 C31 C32 C34 -64.33(16) . . . . ?
C30 C31 C32 C34 115.07(14) . . . . ?
C35 C31 C32 C33 58.69(17) . . . . ?
C30 C31 C32 C33 -121.91(14) . . . . ?
C30 C31 C35 C36 -1.0(2) . . . . ?
C32 C31 C35 C36 178.46(12) . . . . ?
C31 C35 C36 C37 -2.3(2) . . . . ?
C35 C36 C37 C38 2.6(2) . . . . ?
C36 C37 C38 C30 0.4(2) . . . . ?
C36 C37 C38 C39 -177.65(13) . . . . ?
C31 C30 C38 C37 -3.75(19) . . . . ?
N2 C30 C38 C37 166.95(11) . . . . ?
Ca1 C30 C38 C37 117.75(11) . . . . ?
C31 C30 C38 C39 174.36(12) . . . . ?
N2 C30 C38 C39 -14.94(18) . . . . ?
Ca1 C30 C38 C39 -64.15(12) . . . . ?
C37 C38 C39 C40 97.47(15) . . . . ?
C30 C38 C39 C40 -80.59(16) . . . . ?
C37 C38 C39 C41 -26.97(18) . . . . ?
C30 C38 C39 C41 154.97(13) . . . . ?
C47 C42 C43 C44 0.7(3) . . . . ?
C42 C43 C44 C45 0.1(3) . . . . ?
C43 C44 C45 C46 -0.8(3) . . . . ?
C44 C45 C46 C47 0.6(3) . . . . ?
C45 C46 C47 C42 0.2(3) . . . . ?
C43 C42 C47 C46 -0.9(3) . . . . ?
C50 C48 C49 C50 -0.1(3) 2_667 . . . ?
C48 C49 C50 C48 0.1(3) . . . 2_667 ?
