#------------------------------------------------------------------------------
#$Date: 2017-09-07 04:37:53 +0300 (Thu, 07 Sep 2017) $
#$Revision: 200256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/06/7120620.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_7120620
loop_
_publ_author_name
'Causero, Andrea'
'Elsen, Holger'
'Ballmann, Gerd'
'Escalona, Ana'
'Harder, Sjoerd'
_publ_section_title
;
 Calcium stilbene complexes: structures and dual reactivity
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05792J
_journal_year                    2017
_chemical_formula_moiety         'C84 H110 Ca2 N4, 2(C6 H6)'
_chemical_formula_sum            'C96 H122 Ca2 N4'
_chemical_formula_weight         1412.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.776(2)
_cell_angle_beta                 91.061(2)
_cell_angle_gamma                115.639(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3795(3)
_cell_length_b                   10.7062(4)
_cell_length_c                   20.4813(4)
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3280
_cell_measurement_theta_min      4.4290
_cell_volume                     1993.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  32.00   1.00   12.50    --  -41.69  77.00 -30.00  105
  2  ω   -114.00 -19.00   1.00   12.50    --  -41.69 -38.00  60.00   95
  3  ω    -64.00  31.00   1.00   12.50    --  -41.69  38.00-120.00   95
  4  ω     23.00  97.00   1.00   12.50    --   41.69-125.00 120.00   74
  5  ω     94.00 178.00   1.00   50.00    --  106.00 125.00  30.00   84
  6  ω     25.00 109.00   1.00   50.00    --  106.00 -94.00 120.00   84
  7  ω     35.00 130.00   1.00   50.00    --  106.00 -45.00 120.00   95
  8  ω     34.00 121.00   1.00   50.00    --  106.00-125.00  30.00   87
  9  ω     82.00 177.00   1.00   50.00    --  106.00  45.00 150.00   95
 10  ω     82.00 177.00   1.00   50.00    --  106.00  45.00-150.00   95
 11  ω     36.00 134.00   1.00   50.00    --  106.00 -61.00   0.00   98
 12  ω     25.00 109.00   1.00   50.00    --  106.00 -94.00-180.00   84
 13  ω     75.00 178.00   1.00   50.00    --  106.00  77.00  90.00  103
 14  ω   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00-180.00   97
 15  ω   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00   0.00   97
 16  ω   -116.00 -20.00   1.00   12.50    --  -41.69 -77.00 120.00   96
 17  ω   -112.00 -15.00   1.00   12.50    --  -41.69 -57.00 -90.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18091
_diffrn_reflns_point_group_measured_fraction_full 0.995
_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         4.443
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       plate
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0817P)²+0.4017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6399
_reflns_number_total             7259
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc05792j2.cif
_cod_data_source_block           hasj170224b
_cod_original_cell_volume        1993.93(11)
_cod_database_code               7120620
_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.
;
_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:
 C33(H33), C11(H11), C18(H18), C6(H6), C4(H4), C30(H30), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C15(H15), C37(H37), C36(H36), C40(H40), C28(H28),
 C38(H38), C39(H39), C26(H26), C27(H27), C47(H47), C48(H48), C45(H45), C46(H46),
  C43(H43), C44(H44)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-02-24
_olex2_submission_original_sample_id hasj170224b
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
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
Ca1 Ca 0.86108(3) 0.91500(3) 0.88583(2) 0.02005(11) Uani 1 1 d .
N1 N 0.74386(14) 0.71957(15) 0.79059(7) 0.0187(3) Uani 1 1 d .
N2 N 0.53465(15) 0.74377(15) 0.77593(7) 0.0210(3) Uani 1 1 d .
C1 C 0.61136(17) 0.67463(17) 0.75749(8) 0.0178(3) Uani 1 1 d .
C2 C 0.52660(17) 0.53998(18) 0.69975(8) 0.0183(3) Uani 1 1 d .
C3 C 0.38583(17) 0.44615(19) 0.72605(8) 0.0209(3) Uani 1 1 d .
H3A H 0.4099 0.4147 0.7637 0.025 Uiso 1 1 calc R
H3B H 0.3358 0.5027 0.7420 0.025 Uiso 1 1 calc R
C12 C 0.59594(18) 0.86118(19) 0.83021(8) 0.0211(3) Uani 1 1 d .
C24 C 0.84674(17) 0.66930(18) 0.77036(8) 0.0207(3) Uani 1 1 d .
C33 C 0.81331(19) 0.56457(19) 0.87419(9) 0.0247(4) Uani 1 1 d .
H33 H 0.7989 0.6475 0.8955 0.030 Uiso 1 1 calc R
C14 C 0.63918(19) 0.9609(2) 0.95076(9) 0.0258(4) Uani 1 1 d .
H14 H 0.6240 0.9495 0.9942 0.031 Uiso 1 1 calc R
C8 C 0.60085(17) 0.44502(18) 0.67392(8) 0.0210(3) Uani 1 1 d .
H8A H 0.6880 0.4999 0.6559 0.025 Uiso 1 1 calc R
H8B H 0.6277 0.4140 0.7110 0.025 Uiso 1 1 calc R
C11 C 0.50049(18) 0.31387(19) 0.61902(8) 0.0228(4) Uani 1 1 d .
H11 H 0.5502 0.2557 0.6033 0.027 Uiso 1 1 calc R
C29 C 0.88710(18) 0.59849(18) 0.81202(9) 0.0233(4) Uani 1 1 d .
C16 C 0.7456(2) 1.1140(2) 0.87585(10) 0.0300(4) Uani 1 1 d .
H16 H 0.8028 1.2045 0.8695 0.036 Uiso 1 1 calc R
C7 C 0.48192(19) 0.58524(19) 0.63941(8) 0.0238(4) Uani 1 1 d .
H7A H 0.4323 0.6426 0.6545 0.029 Uiso 1 1 calc R
H7B H 0.5673 0.6430 0.6211 0.029 Uiso 1 1 calc R
C15 C 0.7271(2) 1.0951(2) 0.94078(9) 0.0299(4) Uani 1 1 d .
H15 H 0.7735 1.1720 0.9774 0.036 Uiso 1 1 calc R
C18 C 0.47647(18) 0.6956(2) 0.90621(9) 0.0258(4) Uani 1 1 d .
H18 H 0.4956 0.6266 0.8736 0.031 Uiso 1 1 calc R
C6 C 0.3828(2) 0.4540(2) 0.58432(9) 0.0262(4) Uani 1 1 d .
H6 H 0.3571 0.4854 0.5465 0.031 Uiso 1 1 calc R
C25 C 0.92284(18) 0.70625(19) 0.71490(9) 0.0254(4) Uani 1 1 d .
C17 C 0.6798(2) 0.9994(2) 0.81990(9) 0.0266(4) Uani 1 1 d .
C9 C 0.36275(19) 0.22428(19) 0.64662(9) 0.0258(4) Uani 1 1 d .
H9A H 0.3000 0.1421 0.6117 0.031 Uiso 1 1 calc R
H9B H 0.3865 0.1905 0.6834 0.031 Uiso 1 1 calc R
C37 C 1.2450(2) 1.0164(2) 0.84721(9) 0.0328(4) Uani 1 1 d .
H37 H 1.2700 0.9473 0.8242 0.039 Uiso 1 1 calc R
C41 C 1.12369(18) 1.09304(19) 0.93797(8) 0.0239(4) Uani 1 1 d .
C13 C 0.57339(18) 0.84297(19) 0.89655(9) 0.0224(4) Uani 1 1 d .
C4 C 0.28628(18) 0.3159(2) 0.67125(9) 0.0253(4) Uani 1 1 d .
H4 H 0.1988 0.2595 0.6896 0.030 Uiso 1 1 calc R
C10 C 0.46049(19) 0.3636(2) 0.56017(9) 0.0263(4) Uani 1 1 d .
H10A H 0.5469 0.4192 0.5419 0.032 Uiso 1 1 calc R
H10B H 0.3986 0.2816 0.5249 0.032 Uiso 1 1 calc R
C36 C 1.15938(19) 0.9881(2) 0.89935(9) 0.0261(4) Uani 1 1 d .
H36 H 1.1249 0.8988 0.9090 0.031 Uiso 1 1 calc R
C40 C 1.1660(2) 1.2199(2) 0.91430(9) 0.0289(4) Uani 1 1 d .
H40 H 1.1365 1.2877 0.9344 0.035 Uiso 1 1 calc R
C28 C 0.9964(2) 0.5597(2) 0.79477(10) 0.0324(4) Uani 1 1 d .
H28 H 1.0220 0.5106 0.8209 0.039 Uiso 1 1 calc R
C5 C 0.24581(19) 0.3653(2) 0.61248(9) 0.0282(4) Uani 1 1 d .
H5A H 0.1956 0.4221 0.6276 0.034 Uiso 1 1 calc R
H5B H 0.1822 0.2832 0.5777 0.034 Uiso 1 1 calc R
C42 C 1.04049(18) 1.07111(18) 0.99321(9) 0.0224(4) Uani 1 1 d .
C35 C 0.6638(2) 0.4369(2) 0.85685(10) 0.0298(4) Uani 1 1 d .
H35A H 0.6049 0.4552 0.8271 0.045 Uiso 1 1 calc GR
H35B H 0.6200 0.4225 0.8973 0.045 Uiso 1 1 calc GR
H35C H 0.6729 0.3531 0.8353 0.045 Uiso 1 1 calc GR
C30 C 0.89238(19) 0.7935(2) 0.67243(9) 0.0283(4) Uani 1 1 d .
H30 H 0.7977 0.7885 0.6805 0.034 Uiso 1 1 calc R
C38 C 1.2931(2) 1.1455(2) 0.82940(10) 0.0355(5) Uani 1 1 d .
H38 H 1.3534 1.1657 0.7960 0.043 Uiso 1 1 calc R
C39 C 1.2489(2) 1.2447(2) 0.86271(10) 0.0349(4) Uani 1 1 d .
H39 H 1.2764 1.3300 0.8496 0.042 Uiso 1 1 calc R
C26 C 1.0320(2) 0.6664(2) 0.70083(10) 0.0345(5) Uani 1 1 d .
H26 H 1.0819 0.6900 0.6645 0.041 Uiso 1 1 calc R
C19 C 0.3194(2) 0.6639(2) 0.88950(10) 0.0344(4) Uani 1 1 d .
H19A H 0.2981 0.7316 0.9200 0.052 Uiso 1 1 calc GR
H19B H 0.2572 0.5693 0.8938 0.052 Uiso 1 1 calc GR
H19C H 0.3042 0.6708 0.8443 0.052 Uiso 1 1 calc GR
C22 C 0.6937(3) 1.0208(2) 0.74886(10) 0.0364(5) Uani 1 1 d .
H22 H 0.7098 0.9431 0.7220 0.044 Uiso 1 1 calc R
C27 C 1.0676(2) 0.5926(3) 0.73958(11) 0.0408(5) Uani 1 1 d .
H27 H 1.1395 0.5648 0.7288 0.049 Uiso 1 1 calc R
C32 C 0.8881(2) 0.7399(3) 0.59635(10) 0.0399(5) Uani 1 1 d .
H32A H 0.9824 0.7526 0.5863 0.060 Uiso 1 1 calc GR
H32B H 0.8578 0.7930 0.5726 0.060 Uiso 1 1 calc GR
H32C H 0.8216 0.6405 0.5827 0.060 Uiso 1 1 calc GR
C34 C 0.9033(2) 0.5426(2) 0.92678(10) 0.0321(4) Uani 1 1 d .
H34A H 0.9166 0.4595 0.9085 0.048 Uiso 1 1 calc GR
H34B H 0.8543 0.5299 0.9660 0.048 Uiso 1 1 calc GR
H34C H 0.9954 0.6245 0.9388 0.048 Uiso 1 1 calc GR
C20 C 0.5011(2) 0.6742(2) 0.97578(10) 0.0384(5) Uani 1 1 d .
H20A H 0.6009 0.6986 0.9861 0.058 Uiso 1 1 calc GR
H20B H 0.4434 0.5763 0.9766 0.058 Uiso 1 1 calc GR
H20C H 0.4746 0.7343 1.0085 0.058 Uiso 1 1 calc GR
C31 C 1.0032(2) 0.9499(2) 0.69460(12) 0.0434(5) Uani 1 1 d .
H31A H 1.0004 0.9856 0.7413 0.065 Uiso 1 1 calc GR
H31B H 0.9812 1.0045 0.6684 0.065 Uiso 1 1 calc GR
H31C H 1.0976 0.9579 0.6881 0.065 Uiso 1 1 calc GR
C47 C 0.1985(3) -0.3514(3) 0.50649(15) 0.0525(6) Uani 1 1 d .
H47 H 0.1782 -0.4388 0.5161 0.063 Uiso 1 1 calc R
C21 C 0.5514(3) 1.0086(3) 0.71876(11) 0.0509(6) Uani 1 1 d .
H21A H 0.4741 0.9196 0.7219 0.076 Uiso 1 1 calc GR
H21B H 0.5563 1.0129 0.6724 0.076 Uiso 1 1 calc GR
H21C H 0.5346 1.0858 0.7431 0.076 Uiso 1 1 calc GR
C48 C 0.3034(3) -0.2317(3) 0.54522(12) 0.0503(6) Uani 1 1 d .
H48 H 0.3551 -0.2367 0.5814 0.060 Uiso 1 1 calc R
C23 C 0.8189(3) 1.1611(3) 0.74399(13) 0.0569(7) Uani 1 1 d .
H23A H 0.7990 1.2391 0.7642 0.085 Uiso 1 1 calc GR
H23B H 0.8309 1.1610 0.6976 0.085 Uiso 1 1 calc GR
H23C H 0.9056 1.1715 0.7671 0.085 Uiso 1 1 calc GR
C45 C 0.1493(3) -0.2170(4) 0.43976(13) 0.0614(8) Uani 1 1 d .
H45 H 0.0954 -0.2124 0.4044 0.074 Uiso 1 1 calc R
C46 C 0.1216(3) -0.3466(3) 0.45357(14) 0.0560(7) Uani 1 1 d .
H46 H 0.0503 -0.4304 0.4267 0.067 Uiso 1 1 calc R
C43 C 0.3343(3) -0.1036(3) 0.53185(15) 0.0621(8) Uani 1 1 d .
H43 H 0.4077 -0.0210 0.5585 0.075 Uiso 1 1 calc R
C44 C 0.2574(3) -0.0955(3) 0.47884(18) 0.0677(8) Uani 1 1 d .
H44 H 0.2788 -0.0075 0.4696 0.081 Uiso 1 1 calc R
H42 H 1.004(2) 1.140(2) 1.0093(10) 0.026(5) 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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 -6 0.0510
-2 4 -12 0.0358
1 3 9 0.0431
-2 1 -12 0.0288
2 2 -13 0.0354
0 -6 7 0.0682
0 -2 13 0.0378
-5 1 -9 0.0543
0 -1 -12 0.0269
-1 -2 -10 0.0342
5 -5 -6 0.0332
2 -4 -9 0.0309
4 -4 11 0.0401
-1 1 13 0.0263
-4 4 8 0.0363
-6 6 0 0.0417
-4 4 -10 0.0327
3 -2 -11 0.0271
2 5 -6 0.0655
0 1 -13 0.0241
1 -2 13 0.0289
3 -1 12 0.0359
5 -6 5 0.0464
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
N1 Ca1 C12 61.20(5) . .
N1 Ca1 C14 106.50(5) . .
N1 Ca1 C16 105.51(5) . .
N1 Ca1 C15 120.91(5) . .
N1 Ca1 C17 77.30(5) . .
N1 Ca1 C41 137.46(5) . .
N1 Ca1 C13 77.84(5) . .
N1 Ca1 C36 108.76(5) . .
N1 Ca1 C42 158.25(5) . .
N1 Ca1 C42 131.96(5) . 2_777
C12 Ca1 C14 51.56(5) . .
C12 Ca1 C16 50.98(5) . .
C12 Ca1 C15 59.71(5) . .
C12 Ca1 C17 29.43(5) . .
C12 Ca1 C13 29.96(5) . .
C12 Ca1 C36 160.22(5) . .
C14 Ca1 C16 49.43(6) . .
C14 Ca1 C15 27.94(6) . .
C16 Ca1 C15 27.74(5) . .
C17 Ca1 C14 59.08(5) . .
C17 Ca1 C16 28.21(5) . .
C17 Ca1 C15 50.10(5) . .
C17 Ca1 C36 136.19(6) . .
C41 Ca1 C12 150.61(6) . .
C41 Ca1 C14 115.94(6) . .
C41 Ca1 C16 99.93(6) . .
C41 Ca1 C15 97.06(6) . .
C41 Ca1 C17 122.15(6) . .
C41 Ca1 C13 144.63(6) . .
C41 Ca1 C36 29.99(6) . .
C41 Ca1 C42 58.47(5) . 2_777
C13 Ca1 C14 28.69(5) . .
C13 Ca1 C16 59.17(6) . .
C13 Ca1 C15 50.56(5) . .
C13 Ca1 C17 51.92(5) . .
C13 Ca1 C36 169.80(5) . .
C36 Ca1 C14 144.11(5) . .
C36 Ca1 C16 124.17(6) . .
C36 Ca1 C15 126.91(6) . .
C42 Ca1 C12 132.46(5) 2_777 .
C42 Ca1 C12 138.85(5) . .
C42 Ca1 C14 84.32(5) 2_777 .
C42 Ca1 C14 89.22(5) . .
C42 Ca1 C16 115.76(6) 2_777 .
C42 Ca1 C16 96.11(6) . .
C42 Ca1 C15 79.84(5) . .
C42 Ca1 C15 90.57(6) 2_777 .
C42 Ca1 C17 124.27(6) . .
C42 Ca1 C17 140.42(6) 2_777 .
C42 Ca1 C41 31.96(5) . .
C42 Ca1 C13 102.55(5) 2_777 .
C42 Ca1 C13 116.42(5) . .
C42 Ca1 C36 67.24(5) 2_777 .
C42 Ca1 C36 55.00(5) . .
C42 Ca1 C42 32.89(7) . 2_777
C1 N1 Ca1 127.15(11) . .
C1 N1 C24 126.14(14) . .
C24 N1 Ca1 106.35(10) . .
C1 N2 C12 116.64(14) . .
N1 C1 C2 128.27(14) . .
N2 C1 N1 120.14(15) . .
N2 C1 C2 111.49(14) . .
C3 C2 C1 106.73(12) . .
C8 C2 C1 117.66(13) . .
C8 C2 C3 107.38(14) . .
C8 C2 C7 108.38(13) . .
C7 C2 C1 109.14(13) . .
C7 C2 C3 107.06(13) . .
C2 C3 H3A 109.3 . .
C2 C3 H3B 109.3 . .
H3A C3 H3B 107.9 . .
C4 C3 C2 111.67(13) . .
C4 C3 H3A 109.3 . .
C4 C3 H3B 109.3 . .
N2 C12 Ca1 114.83(10) . .
N2 C12 C17 120.52(15) . .
N2 C12 C13 119.81(16) . .
C17 C12 Ca1 79.54(10) . .
C17 C12 C13 119.66(16) . .
C13 C12 Ca1 76.53(9) . .
C29 C24 N1 118.64(15) . .
C29 C24 C25 119.81(15) . .
C25 C24 N1 120.96(16) . .
C29 C33 H33 106.7 . .
C29 C33 C35 112.55(15) . .
C29 C33 C34 113.87(15) . .
C35 C33 H33 106.7 . .
C34 C33 H33 106.7 . .
C34 C33 C35 109.81(15) . .
Ca1 C14 H14 121.5 . .
C15 C14 Ca1 77.90(10) . .
C15 C14 H14 119.5 . .
C15 C14 C13 120.98(17) . .
C13 C14 Ca1 72.25(9) . .
C13 C14 H14 119.5 . .
C2 C8 H8A 109.4 . .
C2 C8 H8B 109.4 . .
H8A C8 H8B 108.0 . .
C11 C8 C2 110.99(13) . .
C11 C8 H8A 109.4 . .
C11 C8 H8B 109.4 . .
C8 C11 H11 109.4 . .
C9 C11 C8 110.42(14) . .
C9 C11 H11 109.4 . .
C10 C11 C8 109.15(14) . .
C10 C11 H11 109.4 . .
C10 C11 C9 109.07(14) . .
C24 C29 C33 121.21(15) . .
C28 C29 C24 118.35(17) . .
C28 C29 C33 120.44(17) . .
Ca1 C16 H16 122.1 . .
C15 C16 Ca1 76.23(11) . .
C15 C16 H16 119.4 . .
C15 C16 C17 121.23(18) . .
C17 C16 Ca1 73.53(10) . .
C17 C16 H16 119.4 . .
C2 C7 H7A 109.5 . .
C2 C7 H7B 109.5 . .
H7A C7 H7B 108.0 . .
C6 C7 C2 110.90(14) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
Ca1 C15 H15 120.9 . .
C14 C15 Ca1 74.17(10) . .
C14 C15 C16 119.80(17) . .
C14 C15 H15 120.1 . .
C16 C15 Ca1 76.03(11) . .
C16 C15 H15 120.1 . .
C13 C18 H18 107.6 . .
C13 C18 C19 108.83(15) . .
C13 C18 C20 114.38(16) . .
C19 C18 H18 107.6 . .
C20 C18 H18 107.6 . .
C20 C18 C19 110.69(15) . .
C7 C6 H6 109.4 . .
C10 C6 C7 109.67(15) . .
C10 C6 H6 109.4 . .
C10 C6 C5 109.50(15) . .
C5 C6 C7 109.55(14) . .
C5 C6 H6 109.4 . .
C24 C25 C30 121.77(15) . .
C26 C25 C24 119.03(18) . .
C26 C25 C30 119.14(17) . .
C12 C17 Ca1 71.02(9) . .
C12 C17 C22 119.70(16) . .
C16 C17 Ca1 78.26(11) . .
C16 C17 C12 118.91(17) . .
C16 C17 C22 121.37(18) . .
C22 C17 Ca1 122.52(13) . .
C11 C9 H9A 109.9 . .
C11 C9 H9B 109.9 . .
H9A C9 H9B 108.3 . .
C4 C9 C11 109.04(15) . .
C4 C9 H9A 109.9 . .
C4 C9 H9B 109.9 . .
C36 C37 H37 119.5 . .
C38 C37 H37 119.5 . .
C38 C37 C36 121.01(19) . .
C36 C41 Ca1 84.24(10) . .
C36 C41 C42 123.67(17) . .
C40 C41 Ca1 109.07(12) . .
C40 C41 C36 115.21(16) . .
C40 C41 C42 120.90(17) . .
C42 C41 Ca1 73.90(10) . .
C12 C13 Ca1 73.51(9) . .
C12 C13 C18 118.80(16) . .
C14 C13 Ca1 79.06(10) . .
C14 C13 C12 119.28(17) . .
C14 C13 C18 121.92(16) . .
C18 C13 Ca1 118.54(11) . .
C3 C4 H4 109.4 . .
C9 C4 C3 109.82(14) . .
C9 C4 H4 109.4 . .
C9 C4 C5 109.44(14) . .
C5 C4 C3 109.40(15) . .
C5 C4 H4 109.4 . .
C11 C10 H10A 109.7 . .
C11 C10 H10B 109.7 . .
C6 C10 C11 109.62(14) . .
C6 C10 H10A 109.7 . .
C6 C10 H10B 109.7 . .
H10A C10 H10B 108.2 . .
Ca1 C36 H36 81.6 . .
C37 C36 Ca1 123.59(13) . .
C37 C36 C41 121.45(18) . .
C37 C36 H36 119.3 . .
C41 C36 Ca1 65.76(9) . .
C41 C36 H36 119.3 . .
C41 C40 H40 119.1 . .
C39 C40 C41 121.83(19) . .
C39 C40 H40 119.1 . .
C29 C28 H28 119.2 . .
C27 C28 C29 121.54(19) . .
C27 C28 H28 119.2 . .
C6 C5 H5A 109.8 . .
C6 C5 H5B 109.8 . .
C4 C5 C6 109.22(14) . .
C4 C5 H5A 109.8 . .
C4 C5 H5B 109.8 . .
H5A C5 H5B 108.3 . .
Ca1 C42 Ca1 147.11(7) . 2_777
Ca1 C42 H42 93.0(12) 2_777 .
Ca1 C42 H42 101.2(12) . .
C41 C42 Ca1 74.14(10) . .
C41 C42 Ca1 125.03(12) . 2_777
C41 C42 C42 122.4(2) . 2_777
C41 C42 H42 116.7(13) . .
C42 C42 Ca1 73.02(13) 2_777 2_777
C42 C42 Ca1 74.10(13) 2_777 .
C42 C42 H42 115.9(13) 2_777 .
C33 C35 H35A 109.5 . .
C33 C35 H35B 109.5 . .
C33 C35 H35C 109.5 . .
H35A C35 H35B 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C25 C30 H30 107.6 . .
C25 C30 C32 114.16(17) . .
C25 C30 C31 110.21(16) . .
C32 C30 H30 107.6 . .
C31 C30 H30 107.6 . .
C31 C30 C32 109.44(17) . .
C37 C38 H38 120.9 . .
C37 C38 C39 118.29(17) . .
C39 C38 H38 120.9 . .
C40 C39 C38 121.73(19) . .
C40 C39 H39 119.1 . .
C38 C39 H39 119.1 . .
C25 C26 H26 119.4 . .
C27 C26 C25 121.28(19) . .
C27 C26 H26 119.4 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C17 C22 H22 107.7 . .
C17 C22 C21 109.11(18) . .
C17 C22 C23 113.93(18) . .
C21 C22 H22 107.7 . .
C23 C22 H22 107.7 . .
C23 C22 C21 110.6(2) . .
C28 C27 H27 120.1 . .
C26 C27 C28 119.88(17) . .
C26 C27 H27 120.1 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32B 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34B 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C18 C20 H20A 109.5 . .
C18 C20 H20B 109.5 . .
C18 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C48 C47 H47 119.5 . .
C48 C47 C46 120.9(3) . .
C46 C47 H47 119.5 . .
C22 C21 H21A 109.5 . .
C22 C21 H21B 109.5 . .
C22 C21 H21C 109.5 . .
H21A C21 H21B 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C47 C48 H48 119.9 . .
C47 C48 C43 120.2(2) . .
C43 C48 H48 119.9 . .
C22 C23 H23A 109.5 . .
C22 C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23B 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C46 C45 H45 120.5 . .
C44 C45 H45 120.5 . .
C44 C45 C46 119.0(2) . .
C47 C46 C45 119.8(2) . .
C47 C46 H46 120.1 . .
C45 C46 H46 120.1 . .
C48 C43 H43 120.0 . .
C48 C43 C44 120.1(3) . .
C44 C43 H43 120.0 . .
C45 C44 C43 119.8(3) . .
C45 C44 H44 120.1 . .
C43 C44 H44 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 N1 2.3887(14) .
Ca1 C12 2.7289(17) .
Ca1 C14 2.8532(17) .
Ca1 C16 2.8973(19) .
Ca1 C15 2.8998(18) .
Ca1 C17 2.8378(18) .
Ca1 C41 2.6017(17) .
Ca1 C13 2.7677(17) .
Ca1 C36 2.8388(18) .
Ca1 C42 2.5986(17) .
Ca1 C42 2.6131(17) 2_777
N1 C1 1.357(2) .
N1 C24 1.423(2) .
N2 C1 1.316(2) .
N2 C12 1.390(2) .
C1 C2 1.555(2) .
C2 C3 1.554(2) .
C2 C8 1.543(2) .
C2 C7 1.548(2) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 C4 1.531(2) .
C12 C17 1.418(3) .
C12 C13 1.421(2) .
C24 C29 1.416(3) .
C24 C25 1.420(2) .
C33 H33 0.9800 .
C33 C29 1.524(3) .
C33 C35 1.532(3) .
C33 C34 1.531(2) .
C14 H14 0.9300 .
C14 C15 1.389(3) .
C14 C13 1.395(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 C11 1.539(2) .
C11 H11 0.9800 .
C11 C9 1.532(2) .
C11 C10 1.531(2) .
C29 C28 1.395(2) .
C16 H16 0.9300 .
C16 C15 1.390(3) .
C16 C17 1.399(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 C6 1.538(2) .
C15 H15 0.9300 .
C18 H18 0.9800 .
C18 C13 1.517(3) .
C18 C19 1.531(2) .
C18 C20 1.523(3) .
C6 H6 0.9800 .
C6 C10 1.526(3) .
C6 C5 1.530(3) .
C25 C30 1.519(3) .
C25 C26 1.389(3) .
C17 C22 1.519(3) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 C4 1.527(3) .
C37 H37 0.9300 .
C37 C36 1.399(3) .
C37 C38 1.381(3) .
C41 C36 1.426(3) .
C41 C40 1.426(3) .
C41 C42 1.432(2) .
C4 H4 0.9800 .
C4 C5 1.529(3) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C36 H36 0.9300 .
C40 H40 0.9300 .
C40 C39 1.370(3) .
C28 H28 0.9300 .
C28 C27 1.384(3) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C42 Ca1 2.6130(17) 2_777
C42 C42 1.475(3) 2_777
C42 H42 0.97(2) .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
C30 H30 0.9800 .
C30 C32 1.540(3) .
C30 C31 1.529(3) .
C38 H38 0.9300 .
C38 C39 1.393(3) .
C39 H39 0.9300 .
C26 H26 0.9300 .
C26 C27 1.374(3) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C22 H22 0.9800 .
C22 C21 1.531(3) .
C22 C23 1.527(3) .
C27 H27 0.9300 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C34 H34A 0.9600 .
C34 H34B 0.9600 .
C34 H34C 0.9600 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C47 H47 0.9300 .
C47 C48 1.343(4) .
C47 C46 1.357(4) .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C48 H48 0.9300 .
C48 C43 1.354(4) .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C45 H45 0.9300 .
C45 C46 1.380(4) .
C45 C44 1.368(4) .
C46 H46 0.9300 .
C43 H43 0.9300 .
C43 C44 1.375(4) .
C44 H44 0.9300 .
