#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:09:43 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/18/7041817.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_7041817
loop_
_publ_author_name
'Causero, Andrea'
'Ballmann, Gerd'
'Pahl, Jürgen'
'Färber, Christian'
'Intemann, Julia'
'Harder, Sjoerd'
_publ_section_title
;
 β-Diketiminate calcium hydride complexes: the importance of solvent
 effects.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1822
_journal_page_last               1831
_journal_paper_doi               10.1039/c6dt04659b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C66 H104 Ca2 N4 O2'
_chemical_formula_sum            'C66 H104 Ca2 N4 O2'
_chemical_formula_weight         1065.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5028(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.98073(15)
_cell_length_b                   15.11446(17)
_cell_length_c                   18.0466(2)
_cell_measurement_reflns_used    7112
_cell_measurement_temperature    291.81(10)
_cell_measurement_theta_max      73.5630
_cell_measurement_theta_min      3.8180
_cell_volume                     3239.94(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.81(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  -90.0000 81

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.00   37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   19.0000 -150.0000 116

#__ type_ start__ end____ width___ exp.time_
  3 omega  -94.00  -56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000 -180.0000 38

#__ type_ start__ end____ width___ exp.time_
  4 omega   39.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  -90.0000 59

#__ type_ start__ end____ width___ exp.time_
  5 omega   50.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 41

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -150.0000 60

#__ type_ start__ end____ width___ exp.time_
  7 omega   31.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
  8 omega   52.00   89.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  150.0000 37

#__ type_ start__ end____ width___ exp.time_
  9 omega   43.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 10 omega   25.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -95.0000  100.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0467746000
_diffrn_orient_matrix_UB_12      0.0234316000
_diffrn_orient_matrix_UB_13      0.0730994000
_diffrn_orient_matrix_UB_21      -0.1169063000
_diffrn_orient_matrix_UB_22      -0.0343142000
_diffrn_orient_matrix_UB_23      -0.0334503000
_diffrn_orient_matrix_UB_31      0.0312056000
_diffrn_orient_matrix_UB_32      -0.0930742000
_diffrn_orient_matrix_UB_33      0.0307768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11551
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         3.828
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.2716
_exptl_crystal_size_mid          0.1884
_exptl_crystal_size_min          0.1097
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0441
_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)+(0.0660P)²+1.0980P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5302
_reflns_number_total             5888
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04659b2.cif
_cod_data_source_block           hasj150130c
_cod_depositor_comments
'Adding full bibliography for 7041815--7041821.cif.'
_cod_original_cell_volume        3239.93(7)
_cod_database_code               7041817
_chemical_oxdiff_formula         'Ca N H C'
_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.
;
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C12(H12), C15(H15), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C10(H10), C21(H21), C8(H8), C9(H9), C20(H20)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C28(H28A,H28B,H28C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C13(H13A,H13B,
 H13C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-01-30
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Ca1 Ca 0.47523(3) 0.58450(2) 0.43075(2) 0.02043(11) Uani 1 1 d .
O1 O 0.29115(11) 0.57049(9) 0.36050(8) 0.0338(3) Uani 1 1 d .
N2 N 0.47142(11) 0.74195(9) 0.43949(7) 0.0188(3) Uani 1 1 d .
N1 N 0.57383(12) 0.62323(9) 0.32919(8) 0.0204(3) Uani 1 1 d .
C3 C 0.47678(14) 0.76360(11) 0.30679(9) 0.0205(3) Uani 1 1 d .
C4 C 0.54307(14) 0.69264(11) 0.28621(9) 0.0208(3) Uani 1 1 d .
C2 C 0.45259(13) 0.79021(10) 0.37786(9) 0.0189(3) Uani 1 1 d .
C22 C 0.84488(16) 0.50998(12) 0.31294(11) 0.0281(4) Uani 1 1 d .
H22 H 0.9198 0.5132 0.3342 0.034 Uiso 1 1 calc R
C23 C 0.76620(15) 0.56731(11) 0.33776(10) 0.0235(4) Uani 1 1 d .
C6 C 0.46719(15) 0.78666(11) 0.50916(9) 0.0218(3) Uani 1 1 d .
C27 C 0.80287(14) 0.63560(11) 0.39806(10) 0.0245(4) Uani 1 1 d .
H27 H 0.7396 0.6445 0.4266 0.029 Uiso 1 1 calc R
C18 C 0.65351(15) 0.56267(11) 0.30459(10) 0.0233(4) Uani 1 1 d .
C12 C 0.67164(16) 0.83639(13) 0.50720(10) 0.0297(4) Uani 1 1 d .
H12 H 0.6607 0.8012 0.4612 0.036 Uiso 1 1 calc R
C7 C 0.56222(15) 0.83379(12) 0.54178(9) 0.0253(4) Uani 1 1 d .
C11 C 0.36979(16) 0.78217(12) 0.54550(9) 0.0264(4) Uani 1 1 d .
C15 C 0.26621(16) 0.73058(13) 0.51295(10) 0.0294(4) Uani 1 1 d .
H15 H 0.2798 0.7076 0.4641 0.035 Uiso 1 1 calc R
C29 C 0.90388(16) 0.60648(14) 0.45316(11) 0.0330(4) Uani 1 1 d .
H29A H 0.8915 0.5476 0.4702 0.050 Uiso 1 1 calc GR
H29B H 0.9132 0.6461 0.4951 0.050 Uiso 1 1 calc GR
H29C H 0.9705 0.6074 0.4288 0.050 Uiso 1 1 calc GR
C1 C 0.40393(16) 0.88266(11) 0.38104(10) 0.0267(4) Uani 1 1 d .
H1A H 0.3427 0.8818 0.4105 0.040 Uiso 1 1 calc GR
H1B H 0.3770 0.9023 0.3313 0.040 Uiso 1 1 calc GR
H1C H 0.4613 0.9223 0.4034 0.040 Uiso 1 1 calc GR
C5 C 0.58068(17) 0.70231(13) 0.20952(10) 0.0295(4) Uani 1 1 d .
H5A H 0.6614 0.7009 0.2142 0.044 Uiso 1 1 calc GR
H5B H 0.5540 0.7576 0.1878 0.044 Uiso 1 1 calc GR
H5C H 0.5504 0.6546 0.1780 0.044 Uiso 1 1 calc GR
C10 C 0.36945(18) 0.82788(14) 0.61273(10) 0.0345(4) Uani 1 1 d .
H10 H 0.3058 0.8254 0.6371 0.041 Uiso 1 1 calc R
C21 C 0.81351(18) 0.44857(13) 0.25743(11) 0.0335(4) Uani 1 1 d .
H21 H 0.8672 0.4118 0.2406 0.040 Uiso 1 1 calc R
C28 C 0.82736(18) 0.72454(13) 0.36315(12) 0.0344(4) Uani 1 1 d .
H28A H 0.8849 0.7170 0.3313 0.052 Uiso 1 1 calc GR
H28B H 0.8525 0.7661 0.4020 0.052 Uiso 1 1 calc GR
H28C H 0.7600 0.7464 0.3343 0.052 Uiso 1 1 calc GR
C19 C 0.62030(17) 0.49775(13) 0.25052(12) 0.0332(4) Uani 1 1 d .
C8 C 0.55670(18) 0.87864(13) 0.60876(10) 0.0324(4) Uani 1 1 d .
H8 H 0.6188 0.9107 0.6303 0.039 Uiso 1 1 calc R
C9 C 0.46080(19) 0.87639(14) 0.64377(10) 0.0366(5) Uani 1 1 d .
H9 H 0.4581 0.9075 0.6880 0.044 Uiso 1 1 calc R
C20 C 0.70234(19) 0.44223(13) 0.22731(12) 0.0364(5) Uani 1 1 d .
H20 H 0.6812 0.4000 0.1906 0.044 Uiso 1 1 calc R
C14 C 0.7036(2) 0.93029(15) 0.48641(15) 0.0453(5) Uani 1 1 d .
H14A H 0.6428 0.9560 0.4536 0.068 Uiso 1 1 calc GR
H14B H 0.7699 0.9283 0.4617 0.068 Uiso 1 1 calc GR
H14C H 0.7184 0.9655 0.5309 0.068 Uiso 1 1 calc GR
C31 C 0.25264(18) 0.61517(14) 0.29090(11) 0.0359(4) Uani 1 1 d .
H31A H 0.2165 0.5722 0.2557 0.043 Uiso 1 1 calc R
H31B H 0.3175 0.6383 0.2703 0.043 Uiso 1 1 calc R
C32 C 0.20621(18) 0.51770(15) 0.38931(12) 0.0380(5) Uani 1 1 d .
H32A H 0.1427 0.5554 0.3959 0.046 Uiso 1 1 calc R
H32B H 0.2367 0.4952 0.4381 0.046 Uiso 1 1 calc R
C17 C 0.16128(18) 0.78973(16) 0.50074(13) 0.0422(5) Uani 1 1 d .
H17A H 0.1438 0.8106 0.5481 0.063 Uiso 1 1 calc GR
H17B H 0.0989 0.7563 0.4764 0.063 Uiso 1 1 calc GR
H17C H 0.1755 0.8393 0.4701 0.063 Uiso 1 1 calc GR
C16 C 0.2459(2) 0.65209(15) 0.56218(13) 0.0444(5) Uani 1 1 d .
H16A H 0.3098 0.6132 0.5661 0.067 Uiso 1 1 calc GR
H16B H 0.1800 0.6207 0.5405 0.067 Uiso 1 1 calc GR
H16C H 0.2352 0.6728 0.6110 0.067 Uiso 1 1 calc GR
C13 C 0.7668(2) 0.79450(18) 0.55942(14) 0.0500(6) Uani 1 1 d .
H13A H 0.7797 0.8281 0.6049 0.075 Uiso 1 1 calc GR
H13B H 0.8340 0.7939 0.5358 0.075 Uiso 1 1 calc GR
H13C H 0.7467 0.7350 0.5706 0.075 Uiso 1 1 calc GR
C33 C 0.1655(2) 0.44228(16) 0.34097(13) 0.0459(5) Uani 1 1 d .
H33A H 0.1287 0.4641 0.2941 0.069 Uiso 1 1 calc GR
H33B H 0.1133 0.4079 0.3651 0.069 Uiso 1 1 calc GR
H33C H 0.2282 0.4058 0.3324 0.069 Uiso 1 1 calc GR
C24 C 0.49898(19) 0.48500(16) 0.21729(15) 0.0511(6) Uani 1 1 d .
H24 H 0.4566 0.5367 0.2309 0.061 Uiso 1 1 calc R
C30 C 0.1719(2) 0.68951(18) 0.29798(14) 0.0536(6) Uani 1 1 d .
H30A H 0.1541 0.7182 0.2504 0.080 Uiso 1 1 calc GR
H30B H 0.2058 0.7315 0.3341 0.080 Uiso 1 1 calc GR
H30C H 0.1043 0.6665 0.3140 0.080 Uiso 1 1 calc GR
C25 C 0.4515(2) 0.4039(2) 0.2528(2) 0.0713(9) Uani 1 1 d .
H25A H 0.4955 0.3528 0.2440 0.107 Uiso 1 1 calc GR
H25B H 0.3749 0.3947 0.2311 0.107 Uiso 1 1 calc GR
H25C H 0.4543 0.4131 0.3057 0.107 Uiso 1 1 calc GR
C26 C 0.4831(3) 0.4787(2) 0.13149(18) 0.0704(9) Uani 1 1 d .
H26A H 0.5190 0.5282 0.1112 0.106 Uiso 1 1 calc GR
H26B H 0.4042 0.4791 0.1131 0.106 Uiso 1 1 calc GR
H26C H 0.5162 0.4248 0.1166 0.106 Uiso 1 1 calc GR
H3 H 0.4558(19) 0.8061(16) 0.2688(13) 0.036(6) Uiso 1 1 d .
H H 0.442(2) 0.4434(19) 0.4568(16) 0.060(8) Uiso 1 1 d .
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 9 -4 0.0847 -1.0097 8.9868 -3.9940 -0.0342 -0.0568 -0.9908
7 -3 3 0.1104 7.0038 -2.9824 3.0056 -0.1778 -0.8170 0.5886
-5 -8 2 0.0540 -4.9918 -8.0000 1.9879 0.1914 0.7916 0.6500
2 -9 -2 0.0837 2.0127 -8.9880 -2.0073 -0.4515 0.1403 0.8375
2 -5 -10 0.0942 2.0114 -4.9961 -10.0066 -0.9426 0.2710 0.2198
-3 9 -2 0.0735 -3.0110 8.9841 -1.9953 0.2055 0.1105 -0.9915
2 6 -9 0.1112 1.9970 5.9930 -8.9957 -0.6106 -0.1382 -0.7723
5 -1 -10 0.0963 5.0069 -0.9947 -9.9997 -0.9885 -0.2167 -0.0590
5 -6 -6 0.0756 5.0114 -5.9875 -6.0029 -0.8135 -0.1796 0.5289
6 5 -6 0.1420 5.9977 5.0030 -5.9913 -0.6013 -0.6724 -0.4629
8 0 -4 0.1294 8.0035 0.0129 -3.9933 -0.6660 -0.8025 0.1256
4 8 -1 0.1270 3.9912 7.9986 -0.9886 -0.0715 -0.7080 -0.6503
-7 -2 -2 0.1227 -6.9979 -2.0119 -2.0100 0.1333 0.9544 -0.0929
5 -6 4 0.1122 5.0067 -5.9825 4.0010 -0.0819 -0.5139 0.8361
6 1 7 0.0873 5.9967 1.0136 7.0099 0.2557 -0.9703 0.3085
3 9 2 0.1041 2.9883 8.9972 2.0125 0.2182 -0.7254 -0.6822
0 7 8 0.0366 -0.0125 6.9967 8.0099 0.7500 -0.5066 -0.4051
-1 10 0 0.0637 -1.0128 9.9878 0.0086 0.2820 -0.2246 -0.9609
-3 7 7 0.0232 -3.0127 6.9907 7.0063 0.8169 -0.1220 -0.5290
-3 9 2 0.0388 -3.0129 8.9861 2.0063 0.4981 -0.0232 -0.8686
-3 5 10 0.0392 -3.0116 4.9942 10.0056 0.9893 -0.1540 -0.2509
-6 3 8 0.0263 -6.0087 2.9897 7.9998 0.9359 0.3323 -0.2195
-7 -2 7 0.0300 -7.0021 -2.0074 6.9936 0.7917 0.6536 0.1836
0 -10 2 0.0818 0.0117 -9.9886 1.9912 -0.0890 0.2748 0.9913
-5 3 -7 0.1391 -5.0015 2.9841 -7.0051 -0.2082 0.7166 -0.6494
4 -3 -10 0.0816 4.0092 -2.9944 -10.0027 -0.9889 -0.0314 0.0959
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
Ca1 Ca1 H 35.5(7) 3_666 .
O1 Ca1 Ca1 111.30(4) . 3_666
O1 Ca1 H 81.5(7) . .
N2 Ca1 Ca1 132.11(4) . 3_666
N2 Ca1 O1 95.65(5) . .
N2 Ca1 H 159.1(7) . .
N1 Ca1 Ca1 131.42(4) . 3_666
N1 Ca1 O1 97.41(5) . .
N1 Ca1 N2 79.70(5) . .
N1 Ca1 H 121.2(7) . .
C31 O1 Ca1 125.64(11) . .
C32 O1 Ca1 120.01(12) . .
C32 O1 C31 114.26(15) . .
C2 N2 Ca1 119.77(10) . .
C2 N2 C6 117.07(13) . .
C6 N2 Ca1 122.08(10) . .
C4 N1 Ca1 121.09(11) . .
C4 N1 C18 117.94(14) . .
C18 N1 Ca1 119.93(10) . .
C4 C3 H3 115.4(14) . .
C2 C3 C4 130.17(15) . .
C2 C3 H3 113.4(14) . .
N1 C4 C3 124.67(15) . .
N1 C4 C5 121.07(15) . .
C3 C4 C5 114.25(15) . .
N2 C2 C3 125.03(15) . .
N2 C2 C1 119.95(14) . .
C3 C2 C1 115.00(14) . .
C23 C22 H22 119.4 . .
C21 C22 H22 119.4 . .
C21 C22 C23 121.22(18) . .
C22 C23 C27 120.40(16) . .
C22 C23 C18 118.92(17) . .
C18 C23 C27 120.65(15) . .
C7 C6 N2 119.12(15) . .
C7 C6 C11 120.19(15) . .
C11 C6 N2 120.67(16) . .
C23 C27 H27 107.4 . .
C23 C27 C29 113.58(15) . .
C23 C27 C28 110.77(15) . .
C29 C27 H27 107.4 . .
C29 C27 C28 110.08(16) . .
C28 C27 H27 107.4 . .
C23 C18 N1 118.52(15) . .
C19 C18 N1 121.43(16) . .
C19 C18 C23 120.01(16) . .
C7 C12 H12 107.8 . .
C7 C12 C14 112.39(16) . .
C14 C12 H12 107.8 . .
C13 C12 H12 107.8 . .
C13 C12 C7 110.55(17) . .
C13 C12 C14 110.31(19) . .
C6 C7 C12 122.31(15) . .
C8 C7 C6 118.80(17) . .
C8 C7 C12 118.88(17) . .
C6 C11 C15 121.89(15) . .
C10 C11 C6 118.41(18) . .
C10 C11 C15 119.70(17) . .
C11 C15 H15 107.9 . .
C11 C15 C17 111.67(16) . .
C11 C15 C16 111.09(17) . .
C17 C15 H15 107.9 . .
C16 C15 H15 107.9 . .
C16 C15 C17 110.36(17) . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29B 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5B 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C11 C10 H10 119.2 . .
C9 C10 C11 121.69(18) . .
C9 C10 H10 119.2 . .
C22 C21 H21 120.3 . .
C20 C21 C22 119.44(17) . .
C20 C21 H21 120.3 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C18 C19 C24 122.38(17) . .
C20 C19 C18 118.77(19) . .
C20 C19 C24 118.84(18) . .
C7 C8 H8 119.3 . .
C9 C8 C7 121.36(19) . .
C9 C8 H8 119.3 . .
C10 C9 C8 119.48(17) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C21 C20 C19 121.51(19) . .
C21 C20 H20 119.2 . .
C19 C20 H20 119.2 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O1 C31 H31A 108.7 . .
O1 C31 H31B 108.7 . .
O1 C31 C30 114.32(18) . .
H31A C31 H31B 107.6 . .
C30 C31 H31A 108.7 . .
C30 C31 H31B 108.7 . .
O1 C32 H32A 108.7 . .
O1 C32 H32B 108.7 . .
O1 C32 C33 114.04(17) . .
H32A C32 H32B 107.6 . .
C33 C32 H32A 108.7 . .
C33 C32 H32B 108.7 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17B 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13B 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C32 C33 H33A 109.5 . .
C32 C33 H33B 109.5 . .
C32 C33 H33C 109.5 . .
H33A C33 H33B 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C19 C24 H24 107.6 . .
C19 C24 C25 109.1(2) . .
C19 C24 C26 113.2(2) . .
C25 C24 H24 107.6 . .
C25 C24 C26 111.6(2) . .
C26 C24 H24 107.6 . .
C31 C30 H30A 109.5 . .
C31 C30 H30B 109.5 . .
C31 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25B 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26B 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 Ca1 3.5689(6) 3_666
Ca1 O1 2.4054(14) .
Ca1 N2 2.3858(14) .
Ca1 N1 2.3796(14) .
Ca1 H 2.23(3) .
O1 C31 1.447(2) .
O1 C32 1.443(2) .
N2 C2 1.325(2) .
N2 C6 1.434(2) .
N1 C4 1.328(2) .
N1 C18 1.434(2) .
C3 C4 1.413(2) .
C3 C2 1.410(2) .
C3 H3 0.95(2) .
C4 C5 1.518(2) .
C2 C1 1.518(2) .
C22 H22 0.9300 .
C22 C23 1.397(2) .
C22 C21 1.381(3) .
C23 C27 1.522(3) .
C23 C18 1.405(3) .
C6 C7 1.405(3) .
C6 C11 1.413(2) .
C27 H27 0.9800 .
C27 C29 1.527(3) .
C27 C28 1.529(2) .
C18 C19 1.404(3) .
C12 H12 0.9800 .
C12 C7 1.524(3) .
C12 C14 1.530(3) .
C12 C13 1.519(3) .
C7 C8 1.395(3) .
C11 C15 1.518(3) .
C11 C10 1.397(3) .
C15 H15 0.9800 .
C15 C17 1.535(3) .
C15 C16 1.521(3) .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C10 H10 0.9300 .
C10 C9 1.375(3) .
C21 H21 0.9300 .
C21 C20 1.375(3) .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C19 C20 1.398(3) .
C19 C24 1.511(3) .
C8 H8 0.9300 .
C8 C9 1.382(3) .
C9 H9 0.9300 .
C20 H20 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C31 C30 1.499(3) .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C32 C33 1.479(3) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C33 H33A 0.9600 .
C33 H33B 0.9600 .
C33 H33C 0.9600 .
C24 H24 0.9800 .
C24 C25 1.528(4) .
C24 C26 1.538(4) .
C30 H30A 0.9600 .
C30 H30B 0.9600 .
C30 H30C 0.9600 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
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
Ca1 O1 C31 C30 -106.18(19)
Ca1 O1 C32 C33 -119.03(18)
Ca1 N2 C2 C3 -26.2(2)
Ca1 N2 C2 C1 155.34(12)
Ca1 N2 C6 C7 110.02(15)
Ca1 N2 C6 C11 -68.76(18)
Ca1 N1 C4 C3 19.9(2)
Ca1 N1 C4 C5 -161.61(13)
Ca1 N1 C18 C23 -89.39(17)
Ca1 N1 C18 C19 88.38(18)
N2 C6 C7 C12 -2.3(2)
N2 C6 C7 C8 178.68(15)
N2 C6 C11 C15 -0.1(3)
N2 C6 C11 C10 -179.15(16)
N1 C18 C19 C20 178.26(17)
N1 C18 C19 C24 -2.6(3)
C4 N1 C18 C23 102.16(19)
C4 N1 C18 C19 -80.1(2)
C4 C3 C2 N2 -13.8(3)
C4 C3 C2 C1 164.70(17)
C2 N2 C6 C7 -81.94(19)
C2 N2 C6 C11 99.28(19)
C2 C3 C4 N1 17.7(3)
C2 C3 C4 C5 -160.83(17)
C22 C23 C27 C29 -30.2(2)
C22 C23 C27 C28 94.28(19)
C22 C23 C18 N1 -178.53(15)
C22 C23 C18 C19 3.7(3)
C22 C21 C20 C19 1.3(3)
C23 C22 C21 C20 -1.6(3)
C23 C18 C19 C20 -4.0(3)
C23 C18 C19 C24 175.2(2)
C6 N2 C2 C3 165.44(16)
C6 N2 C2 C1 -13.0(2)
C6 C7 C8 C9 1.0(3)
C6 C11 C15 C17 -122.24(19)
C6 C11 C15 C16 114.08(19)
C6 C11 C10 C9 0.0(3)
C27 C23 C18 N1 -0.4(2)
C27 C23 C18 C19 -178.24(16)
C18 N1 C4 C3 -171.76(16)
C18 N1 C4 C5 6.7(2)
C18 C23 C27 C29 151.73(16)
C18 C23 C27 C28 -83.79(19)
C18 C19 C20 C21 1.5(3)
C18 C19 C24 C25 -103.1(2)
C18 C19 C24 C26 131.9(2)
C12 C7 C8 C9 -178.06(18)
C7 C6 C11 C15 -178.83(16)
C7 C6 C11 C10 2.1(3)
C7 C8 C9 C10 1.1(3)
C11 C6 C7 C12 176.46(16)
C11 C6 C7 C8 -2.5(3)
C11 C10 C9 C8 -1.5(3)
C15 C11 C10 C9 -179.14(18)
C10 C11 C15 C17 56.8(2)
C10 C11 C15 C16 -66.8(2)
C21 C22 C23 C27 -178.93(16)
C21 C22 C23 C18 -0.8(3)
C20 C19 C24 C25 76.1(3)
C20 C19 C24 C26 -48.9(3)
C14 C12 C7 C6 119.0(2)
C14 C12 C7 C8 -62.0(2)
C31 O1 C32 C33 64.2(2)
C32 O1 C31 C30 70.4(2)
C13 C12 C7 C6 -117.2(2)
C13 C12 C7 C8 61.8(2)
C24 C19 C20 C21 -177.7(2)
