#------------------------------------------------------------------------------
#$Date: 2019-11-26 08:00:03 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243003 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/31/4133167.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_4133167
loop_
_publ_author_name
'Werner, Daniel'
'Anwander, Reiner'
_publ_section_title
;
 Unveiling the Takai Olefination Reagent via Tris( tert-butoxy)siloxy
 Variants.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14334
_journal_page_last               14341
_journal_paper_doi               10.1021/jacs.8b08739
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C49 H109 Cr2 I2 O16 Si4, C3 H7'
_chemical_formula_sum            'C52 H116 Cr2 I2 O16 Si4'
_chemical_formula_weight         1467.61
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                94.5434(14)
_cell_angle_beta                 107.6252(14)
_cell_angle_gamma                93.1097(14)
_cell_formula_units_Z            2
_cell_length_a                   13.6739(4)
_cell_length_b                   14.7859(4)
_cell_length_c                   19.0519(5)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.334
_cell_measurement_theta_min      2.748
_cell_volume                     3647.15(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            117347
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0507 before and 0.0421 after correction. The Ratio of minimum to maximum transmission is 0.9240. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.013
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         18203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0257P)²+5.7736P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                15509
_reflns_number_total             18203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b08739_si_006.cif
_cod_data_source_block           5b
_cod_original_cell_volume        3647.15(17)
_cod_database_code               4133167
_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:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B), C100(H10A,H10B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C29(H29A,H29B,
 H29C), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C16(H16A,
 H16B,H16C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C),
 C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C),
  C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C23(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C40(H40A,H40B,H40C), C82(H82A,H82B,H82C), C15(H15A,
 H15B,H15C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C43(H43A,H43B,H43C),
 C49(H49A,H49B,H49C), C45(H45A,H45B,H45C), C12(H12A,H12B,H12C), C36(H36A,H36B,
 H36C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C), C8(H8A,H8B,H8C),
 C44(H44A,H44B,H44C), C20(H20A,H20B,H20C), C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
I2 I 0.339972(11) 0.744293(9) 0.391263(7) 0.01725(4) Uani 1 d A 1 .
I1 I 0.587315(11) 0.776903(10) 0.367308(8) 0.01944(4) Uani 1 d A 1 .
Cr1 Cr 0.40636(2) 0.77827(2) 0.227208(17) 0.01014(6) Uani 1 d . . .
Cr2 Cr 0.23368(2) 0.64746(2) 0.236602(17) 0.01090(6) Uani 1 d . . .
Si2 Si 0.40311(4) 0.59859(4) 0.15902(3) 0.01064(10) Uani 1 d A . .
Si1 Si 0.50928(4) 0.99149(4) 0.23453(3) 0.01272(11) Uani 1 d . . .
Si4 Si 0.17940(4) 0.48886(4) 0.33999(3) 0.01345(11) Uani 1 d . . .
Si3 Si 0.14543(4) 0.80930(4) 0.19207(3) 0.01380(11) Uani 1 d A . .
O9 O 0.25649(11) 0.77319(9) 0.19700(8) 0.0129(3) Uani 1 d A . .
O13 O 0.20124(11) 0.53511(9) 0.27356(8) 0.0144(3) Uani 1 d A . .
O5 O 0.38132(11) 0.64100(9) 0.23323(7) 0.0114(3) Uani 1 d A . .
O6 O 0.43969(11) 0.69723(9) 0.13436(8) 0.0136(3) Uani 1 d A . .
O10 O 0.09139(11) 0.70951(10) 0.20312(8) 0.0148(3) Uani 1 d A . .
O1 O 0.46076(11) 0.88894(9) 0.20795(8) 0.0142(3) Uani 1 d A . .
O3 O 0.42942(12) 1.06496(10) 0.19674(8) 0.0170(3) Uani 1 d A . .
O7 O 0.48788(11) 0.52565(10) 0.16716(8) 0.0151(3) Uani 1 d . . .
O8 O 0.29878(11) 0.55827(9) 0.09531(8) 0.0153(3) Uani 1 d . . .
O2 O 0.52895(13) 1.00466(10) 0.32333(8) 0.0214(3) Uani 1 d A . .
O15 O 0.24741(12) 0.40333(10) 0.36662(9) 0.0185(3) Uani 1 d A . .
O16 O 0.06045(12) 0.44481(10) 0.32111(9) 0.0189(3) Uani 1 d A . .
O14 O 0.19660(12) 0.56836(10) 0.40892(8) 0.0181(3) Uani 1 d A . .
O11 O 0.13870(12) 0.87816(10) 0.25957(9) 0.0201(3) Uani 1 d . . .
O12 O 0.08528(12) 0.84953(10) 0.11606(9) 0.0190(3) Uani 1 d . . .
O4 O 0.61092(12) 1.01596(11) 0.21056(10) 0.0251(4) Uani 1 d A . .
C1 C 0.43018(16) 0.81433(14) 0.33740(12) 0.0174(4) Uani 1 d A 1 .
H1 H 0.4287 0.8816 0.3471 0.021 Uiso 1 calc A 1 R
C4 C 0.6575(2) 1.05348(17) 0.43810(13) 0.0281(5) Uani 1 d A . .
H4A H 0.6455 0.9938 0.4544 0.042 Uiso 1 calc . . GR
H4B H 0.6780 1.0996 0.4809 0.042 Uiso 1 calc . . GR
H4C H 0.7123 1.0514 0.4149 0.042 Uiso 1 calc . . GR
C30 C 0.14980(18) 0.97668(14) 0.27427(14) 0.0225(5) Uani 1 d A . .
C48 C -0.1026(2) 0.36887(19) 0.26020(17) 0.0357(6) Uani 1 d A . .
H48A H -0.1237 0.3901 0.3030 0.053 Uiso 1 calc . . GR
H48B H -0.1405 0.3103 0.2377 0.053 Uiso 1 calc . . GR
H48C H -0.1176 0.4136 0.2239 0.053 Uiso 1 calc . . GR
C14 C 0.46228(17) 0.71830(14) 0.06625(11) 0.0161(4) Uani 1 d . . .
C6 C 0.41569(18) 1.10949(14) 0.13037(12) 0.0197(4) Uani 1 d . . .
C26 C -0.01033(16) 0.68864(15) 0.21361(12) 0.0174(4) Uani 1 d . . .
C47 C 0.0488(2) 0.32998(18) 0.21882(15) 0.0317(6) Uani 1 d A . .
H47A H 0.0358 0.3775 0.1848 0.048 Uiso 1 calc . . GR
H47B H 0.0114 0.2725 0.1930 0.048 Uiso 1 calc . . GR
H47C H 0.1227 0.3223 0.2361 0.048 Uiso 1 calc . . GR
C34 C 0.07424(18) 0.82614(15) 0.03878(13) 0.0215(5) Uani 1 d A . .
C22 C 0.24374(16) 0.46914(14) 0.07069(12) 0.0157(4) Uani 1 d A . .
C42 C 0.35543(17) 0.39126(15) 0.38395(12) 0.0198(4) Uani 1 d . . .
C29 C -0.08696(17) 0.75288(16) 0.17336(14) 0.0246(5) Uani 1 d A . .
H29A H -0.0629 0.8158 0.1943 0.037 Uiso 1 calc . . GR
H29B H -0.1544 0.7375 0.1793 0.037 Uiso 1 calc . . GR
H29C H -0.0928 0.7466 0.1206 0.037 Uiso 1 calc . . GR
C18 C 0.58977(16) 0.51681(14) 0.21760(12) 0.0168(4) Uani 1 d A . .
C19 C 0.66240(18) 0.59876(17) 0.21871(14) 0.0243(5) Uani 1 d . . .
H19A H 0.6677 0.6030 0.1689 0.036 Uiso 1 calc A . GR
H19B H 0.7306 0.5919 0.2531 0.036 Uiso 1 calc . . GR
H19C H 0.6357 0.6542 0.2349 0.036 Uiso 1 calc . . GR
C46 C 0.01203(18) 0.35749(15) 0.28506(14) 0.0228(5) Uani 1 d . . .
C38 C 0.17379(18) 0.56749(16) 0.47825(12) 0.0213(5) Uani 1 d . . .
C27 C -0.04328(17) 0.59117(15) 0.18020(13) 0.0211(4) Uani 1 d A . .
H27A H -0.0484 0.5864 0.1276 0.032 Uiso 1 calc . . GR
H27B H -0.1104 0.5729 0.1855 0.032 Uiso 1 calc . . GR
H27C H 0.0077 0.5511 0.2059 0.032 Uiso 1 calc . . GR
C32 C 0.0486(2) 1.01272(19) 0.2337(2) 0.0463(8) Uani 1 d . . .
H32A H 0.0330 0.9966 0.1804 0.069 Uiso 1 calc A . GR
H32B H 0.0538 1.0791 0.2441 0.069 Uiso 1 calc . . GR
H32C H -0.0065 0.9857 0.2504 0.069 Uiso 1 calc . . GR
C16 C 0.56252(19) 0.77797(16) 0.09028(13) 0.0233(5) Uani 1 d A . .
H16A H 0.5555 0.8326 0.1204 0.035 Uiso 1 calc . . GR
H16B H 0.5792 0.7957 0.0465 0.035 Uiso 1 calc . . GR
H16C H 0.6178 0.7442 0.1195 0.035 Uiso 1 calc . . GR
C25 C 0.13068(18) 0.48627(16) 0.04526(14) 0.0252(5) Uani 1 d . . .
H25A H 0.1116 0.5142 0.0871 0.038 Uiso 1 calc A . GR
H25B H 0.0891 0.4284 0.0262 0.038 Uiso 1 calc . . GR
H25C H 0.1182 0.5273 0.0060 0.038 Uiso 1 calc . . GR
C2 C 0.55921(18) 1.07773(14) 0.38246(12) 0.0197(4) Uani 1 d . . .
C10 C 0.71772(17) 1.00053(16) 0.22559(13) 0.0212(4) Uani 1 d . . .
C28 C 0.00567(19) 0.69919(18) 0.29625(13) 0.0264(5) Uani 1 d A . .
H28A H 0.0585 0.6600 0.3208 0.040 Uiso 1 calc . . GR
H28B H -0.0591 0.6816 0.3055 0.040 Uiso 1 calc . . GR
H28C H 0.0280 0.7628 0.3158 0.040 Uiso 1 calc . . GR
C35 C 0.0934(2) 0.72669(15) 0.02488(13) 0.0249(5) Uani 1 d . . .
H35A H 0.1644 0.7170 0.0527 0.037 Uiso 1 calc A . GR
H35B H 0.0822 0.7113 -0.0281 0.037 Uiso 1 calc . . GR
H35C H 0.0458 0.6877 0.0411 0.037 Uiso 1 calc . . GR
C5 C 0.4729(2) 1.08099(17) 0.41698(14) 0.0284(5) Uani 1 d A . .
H5A H 0.4104 1.0974 0.3806 0.043 Uiso 1 calc . . GR
H5B H 0.4928 1.1266 0.4601 0.043 Uiso 1 calc . . GR
H5C H 0.4598 1.0211 0.4326 0.043 Uiso 1 calc . . GR
C33 C 0.1750(3) 0.99560(19) 0.35731(16) 0.0393(7) Uani 1 d . . .
H33A H 0.1186 0.9690 0.3729 0.059 Uiso 1 calc A . GR
H33B H 0.1838 1.0615 0.3710 0.059 Uiso 1 calc . . GR
H33C H 0.2388 0.9685 0.3818 0.059 Uiso 1 calc . . GR
C31 C 0.2365(2) 1.01383(17) 0.24840(15) 0.0304(5) Uani 1 d . . .
H31A H 0.2994 0.9852 0.2723 0.046 Uiso 1 calc A . GR
H31B H 0.2479 1.0798 0.2615 0.046 Uiso 1 calc . . GR
H31C H 0.2184 1.0006 0.1946 0.046 Uiso 1 calc . . GR
C39 C 0.2497(2) 0.6389(2) 0.53229(14) 0.0362(7) Uani 1 d A . .
H39A H 0.3201 0.6237 0.5371 0.054 Uiso 1 calc . . GR
H39B H 0.2383 0.6402 0.5807 0.054 Uiso 1 calc . . GR
H39C H 0.2394 0.6988 0.5138 0.054 Uiso 1 calc . . GR
C24 C 0.26594(19) 0.40887(15) 0.13361(13) 0.0222(5) Uani 1 d . . .
H24A H 0.3394 0.3990 0.1497 0.033 Uiso 1 calc A . GR
H24B H 0.2254 0.3502 0.1166 0.033 Uiso 1 calc . . GR
H24C H 0.2474 0.4385 0.1751 0.033 Uiso 1 calc . . GR
C17 C 0.4717(2) 0.63109(16) 0.02181(13) 0.0235(5) Uani 1 d A . .
H17A H 0.5259 0.5973 0.0523 0.035 Uiso 1 calc . . GR
H17B H 0.4893 0.6461 -0.0223 0.035 Uiso 1 calc . . GR
H17C H 0.4061 0.5936 0.0068 0.035 Uiso 1 calc . . GR
C69 C 0.0244(2) 0.1316(2) 0.50031(19) 0.0448(7) Uani 1 d . . .
H69A H -0.0357 0.1503 0.5149 0.054 Uiso 1 calc . . R
H69B H 0.0069 0.1323 0.4460 0.054 Uiso 1 calc . . R
C7 C 0.3083(2) 1.14291(18) 0.11141(16) 0.0332(6) Uani 1 d A . .
H7A H 0.2571 1.0907 0.1020 0.050 Uiso 1 calc . . GR
H7B H 0.2955 1.1756 0.0671 0.050 Uiso 1 calc . . GR
H7C H 0.3032 1.1839 0.1529 0.050 Uiso 1 calc . . GR
C23 C 0.2774(2) 0.42820(17) 0.00686(14) 0.0274(5) Uani 1 d . . .
H23A H 0.2604 0.4675 -0.0335 0.041 Uiso 1 calc A . GR
H23B H 0.2416 0.3676 -0.0108 0.041 Uiso 1 calc . . GR
H23C H 0.3519 0.4232 0.0238 0.041 Uiso 1 calc . . GR
C21 C 0.5815(2) 0.50612(18) 0.29390(13) 0.0264(5) Uani 1 d . . .
H21A H 0.5541 0.5603 0.3115 0.040 Uiso 1 calc A . GR
H21B H 0.6498 0.4988 0.3280 0.040 Uiso 1 calc . . GR
H21C H 0.5351 0.4523 0.2917 0.040 Uiso 1 calc . . GR
C40 C 0.0641(2) 0.59301(19) 0.46572(15) 0.0313(6) Uani 1 d A . .
H40A H 0.0580 0.6543 0.4495 0.047 Uiso 1 calc . . GR
H40B H 0.0468 0.5918 0.5120 0.047 Uiso 1 calc . . GR
H40C H 0.0166 0.5494 0.4276 0.047 Uiso 1 calc . . GR
C82 C 0.1158(3) 0.2004(2) 0.53770(19) 0.0477(8) Uani 1 d . . .
H82A H 0.1743 0.1848 0.5208 0.072 Uiso 1 calc . . GR
H82B H 0.1347 0.1992 0.5915 0.072 Uiso 1 calc . . GR
H82C H 0.0974 0.2614 0.5249 0.072 Uiso 1 calc . . GR
C15 C 0.3749(2) 0.76916(19) 0.02298(14) 0.0298(6) Uani 1 d A . .
H15A H 0.3109 0.7293 0.0080 0.045 Uiso 1 calc . . GR
H15B H 0.3895 0.7883 -0.0212 0.045 Uiso 1 calc . . GR
H15C H 0.3675 0.8229 0.0540 0.045 Uiso 1 calc . . GR
C11 C 0.7375(2) 0.98801(18) 0.15097(14) 0.0282(5) Uani 1 d A . .
H11A H 0.6969 0.9334 0.1220 0.042 Uiso 1 calc . . GR
H11B H 0.8108 0.9813 0.1589 0.042 Uiso 1 calc . . GR
H11C H 0.7174 1.0413 0.1241 0.042 Uiso 1 calc . . GR
C13 C 0.74314(19) 0.91748(16) 0.26781(13) 0.0241(5) Uani 1 d A . .
H13A H 0.7295 0.9274 0.3153 0.036 Uiso 1 calc . . GR
H13B H 0.8160 0.9075 0.2766 0.036 Uiso 1 calc . . GR
H13C H 0.7003 0.8639 0.2387 0.036 Uiso 1 calc . . GR
C43 C 0.41869(18) 0.48276(17) 0.40273(13) 0.0242(5) Uani 1 d A . .
H43A H 0.4010 0.5173 0.3594 0.036 Uiso 1 calc . . GR
H43B H 0.4921 0.4729 0.4170 0.036 Uiso 1 calc . . GR
H43C H 0.4036 0.5170 0.4439 0.036 Uiso 1 calc . . GR
C49 C 0.0357(2) 0.28650(16) 0.34075(15) 0.0296(5) Uani 1 d A . .
H49A H 0.1100 0.2806 0.3578 0.044 Uiso 1 calc . . GR
H49B H -0.0004 0.2277 0.3170 0.044 Uiso 1 calc . . GR
H49C H 0.0126 0.3057 0.3831 0.044 Uiso 1 calc . . GR
C45 C 0.3829(2) 0.33497(19) 0.45013(15) 0.0327(6) Uani 1 d A . .
H45A H 0.3750 0.3704 0.4935 0.049 Uiso 1 calc . . GR
H45B H 0.4544 0.3195 0.4607 0.049 Uiso 1 calc . . GR
H45C H 0.3369 0.2789 0.4387 0.049 Uiso 1 calc . . GR
C12 C 0.7815(2) 1.08533(18) 0.27105(16) 0.0317(6) Uani 1 d A . .
H12A H 0.7602 1.1391 0.2452 0.048 Uiso 1 calc . . GR
H12B H 0.8547 1.0791 0.2774 0.048 Uiso 1 calc . . GR
H12C H 0.7707 1.0921 0.3197 0.048 Uiso 1 calc . . GR
C36 C 0.1510(2) 0.89006(17) 0.01949(16) 0.0326(6) Uani 1 d . . .
H36A H 0.1343 0.9531 0.0267 0.049 Uiso 1 calc A . GR
H36B H 0.1476 0.8752 -0.0323 0.049 Uiso 1 calc . . GR
H36C H 0.2207 0.8831 0.0517 0.049 Uiso 1 calc . . GR
C100 C 0.0439(2) 0.0353(2) 0.51965(15) 0.0340(6) Uani 1 d . . .
H10A H 0.1063 0.0181 0.5075 0.041 Uiso 1 calc . . R
H10B H 0.0582 0.0344 0.5737 0.041 Uiso 1 calc . . R
C3 C 0.5749(2) 1.16880(15) 0.35340(14) 0.0258(5) Uani 1 d A . .
H3A H 0.6310 1.1667 0.3314 0.039 Uiso 1 calc . . GR
H3B H 0.5924 1.2173 0.3943 0.039 Uiso 1 calc . . GR
H3C H 0.5114 1.1809 0.3158 0.039 Uiso 1 calc . . GR
C9 C 0.4955(2) 1.19059(16) 0.14636(14) 0.0304(6) Uani 1 d A . .
H9A H 0.4902 1.2307 0.1883 0.046 Uiso 1 calc . . GR
H9B H 0.4831 1.2243 0.1026 0.046 Uiso 1 calc . . GR
H9C H 0.5646 1.1690 0.1584 0.046 Uiso 1 calc . . GR
C41 C 0.1871(2) 0.47512(17) 0.50851(14) 0.0272(5) Uani 1 d A . .
H41A H 0.1400 0.4286 0.4730 0.041 Uiso 1 calc . . GR
H41B H 0.1717 0.4775 0.5556 0.041 Uiso 1 calc . . GR
H41C H 0.2583 0.4598 0.5165 0.041 Uiso 1 calc . . GR
C8 C 0.4241(2) 1.04344(16) 0.06742(13) 0.0276(5) Uani 1 d A . .
H8A H 0.4938 1.0230 0.0800 0.041 Uiso 1 calc . . GR
H8B H 0.4100 1.0740 0.0220 0.041 Uiso 1 calc . . GR
H8C H 0.3741 0.9908 0.0597 0.041 Uiso 1 calc . . GR
C44 C 0.3715(2) 0.33833(17) 0.31722(14) 0.0280(5) Uani 1 d A . .
H44A H 0.3289 0.2804 0.3058 0.042 Uiso 1 calc . . GR
H44B H 0.4442 0.3265 0.3282 0.042 Uiso 1 calc . . GR
H44C H 0.3518 0.3740 0.2746 0.042 Uiso 1 calc . . GR
C20 C 0.6254(2) 0.43109(18) 0.18656(16) 0.0315(6) Uani 1 d . . .
H20A H 0.5746 0.3797 0.1815 0.047 Uiso 1 calc A . GR
H20B H 0.6919 0.4182 0.2203 0.047 Uiso 1 calc . . GR
H20C H 0.6328 0.4402 0.1380 0.047 Uiso 1 calc . . GR
C37 C -0.0356(2) 0.8434(2) -0.00399(15) 0.0366(6) Uani 1 d . . .
H37A H -0.0839 0.8008 0.0083 0.055 Uiso 1 calc A . GR
H37B H -0.0451 0.8344 -0.0572 0.055 Uiso 1 calc . . GR
H37C H -0.0485 0.9059 0.0094 0.055 Uiso 1 calc . . GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
C1 I2 Cr2 83.77(6) .
C1 I1 Cr1 42.20(6) .
Si2 Cr1 I1 100.597(14) .
O9 Cr1 I1 139.27(4) .
O9 Cr1 Si2 92.06(4) .
O9 Cr1 O5 83.11(6) .
O9 Cr1 O6 103.84(6) .
O9 Cr1 C1 96.61(7) .
O5 Cr1 I1 86.41(4) .
O5 Cr1 Si2 33.74(4) .
O5 Cr1 O6 69.24(5) .
O6 Cr1 I1 108.90(4) .
O6 Cr1 Si2 35.59(4) .
O1 Cr1 I1 90.64(5) .
O1 Cr1 Si2 129.76(5) .
O1 Cr1 O9 110.52(6) .
O1 Cr1 O5 161.29(6) .
O1 Cr1 O6 94.42(6) .
O1 Cr1 C1 95.99(7) .
C1 Cr1 I1 45.28(6) .
C1 Cr1 Si2 126.27(6) .
C1 Cr1 O5 95.02(7) .
C1 Cr1 O6 152.09(7) .
Si3 Cr2 I2 89.569(15) .
O9 Cr2 I2 86.20(4) .
O9 Cr2 Si3 34.70(4) .
O9 Cr2 O10 70.17(5) .
O13 Cr2 I2 93.77(4) .
O13 Cr2 Si3 140.30(5) .
O13 Cr2 O9 174.98(6) .
O13 Cr2 O5 105.29(6) .
O13 Cr2 O10 104.98(6) .
O5 Cr2 I2 83.44(4) .
O5 Cr2 Si3 114.39(4) .
O5 Cr2 O9 79.70(5) .
O5 Cr2 O10 148.60(6) .
O10 Cr2 I2 102.72(4) .
O10 Cr2 Si3 36.31(4) .
O5 Si2 Cr1 44.97(5) .
O5 Si2 O6 96.15(7) .
O6 Si2 Cr1 51.33(5) .
O7 Si2 Cr1 133.45(6) .
O7 Si2 O5 118.19(8) .
O7 Si2 O6 113.00(8) .
O7 Si2 O8 109.07(8) .
O8 Si2 Cr1 117.40(6) .
O8 Si2 O5 112.45(8) .
O8 Si2 O6 106.98(8) .
O1 Si1 O3 111.64(8) .
O1 Si1 O2 105.83(8) .
O1 Si1 O4 113.41(9) .
O2 Si1 O3 108.03(8) .
O4 Si1 O3 104.09(8) .
O4 Si1 O2 113.85(9) .
O13 Si4 O15 114.89(8) .
O13 Si4 O16 113.66(8) .
O13 Si4 O14 107.87(8) .
O15 Si4 O16 103.13(8) .
O15 Si4 O14 111.11(8) .
O16 Si4 O14 105.82(8) .
O9 Si3 Cr2 47.83(5) .
O9 Si3 O10 95.75(7) .
O10 Si3 Cr2 49.23(5) .
O11 Si3 Cr2 113.58(6) .
O11 Si3 O9 117.36(8) .
O11 Si3 O10 105.20(8) .
O11 Si3 O12 107.95(8) .
O12 Si3 Cr2 137.92(6) .
O12 Si3 O9 116.27(8) .
O12 Si3 O10 113.37(8) .
Cr1 O9 Cr2 96.59(6) .
Si3 O9 Cr1 156.17(9) .
Si3 O9 Cr2 97.47(7) .
Si4 O13 Cr2 146.54(9) .
Cr2 O5 Cr1 95.05(6) .
Si2 O5 Cr1 101.28(7) .
Si2 O5 Cr2 120.48(8) .
Si2 O6 Cr1 93.08(6) .
C14 O6 Cr1 135.33(12) .
C14 O6 Si2 130.32(12) .
Si3 O10 Cr2 94.46(7) .
C26 O10 Cr2 132.71(12) .
C26 O10 Si3 129.09(12) .
Si1 O1 Cr1 150.62(9) .
C6 O3 Si1 131.88(14) .
C18 O7 Si2 135.85(13) .
C22 O8 Si2 135.62(13) .
C2 O2 Si1 137.96(14) .
C42 O15 Si4 132.91(14) .
C46 O16 Si4 130.89(15) .
C38 O14 Si4 131.46(14) .
C30 O11 Si3 133.57(15) .
C34 O12 Si3 134.65(14) .
C10 O4 Si1 143.49(15) .
I2 C1 I1 112.85(9) .
Cr1 C1 I2 118.62(9) .
Cr1 C1 I1 92.52(9) .
O11 C30 C32 108.14(19) .
O11 C30 C33 105.4(2) .
O11 C30 C31 108.94(18) .
C33 C30 C32 111.6(2) .
C31 C30 C32 111.4(2) .
C31 C30 C33 111.1(2) .
O6 C14 C16 106.70(17) .
O6 C14 C17 110.24(17) .
O6 C14 C15 106.94(17) .
C16 C14 C17 110.87(19) .
C15 C14 C16 110.9(2) .
C15 C14 C17 111.1(2) .
O3 C6 C7 105.93(19) .
O3 C6 C9 108.97(18) .
O3 C6 C8 110.83(17) .
C7 C6 C9 109.6(2) .
C7 C6 C8 110.2(2) .
C8 C6 C9 111.2(2) .
O10 C26 C29 109.95(17) .
O10 C26 C27 105.33(16) .
O10 C26 C28 107.15(17) .
C27 C26 C29 110.62(19) .
C27 C26 C28 111.98(19) .
C28 C26 C29 111.55(19) .
O12 C34 C35 110.67(18) .
O12 C34 C36 106.78(19) .
O12 C34 C37 106.2(2) .
C36 C34 C35 111.7(2) .
C36 C34 C37 110.6(2) .
C37 C34 C35 110.7(2) .
O8 C22 C25 105.45(16) .
O8 C22 C24 110.68(17) .
O8 C22 C23 107.65(18) .
C25 C22 C24 110.55(19) .
C25 C22 C23 111.22(19) .
C24 C22 C23 111.10(19) .
O15 C42 C43 110.82(17) .
O15 C42 C45 106.61(19) .
O15 C42 C44 107.56(18) .
C43 C42 C45 110.7(2) .
C44 C42 C43 111.2(2) .
C44 C42 C45 109.8(2) .
O7 C18 C19 110.45(17) .
O7 C18 C21 109.08(17) .
O7 C18 C20 105.05(17) .
C19 C18 C20 110.1(2) .
C21 C18 C19 111.27(19) .
C21 C18 C20 110.7(2) .
O16 C46 C48 105.47(19) .
O16 C46 C47 110.79(19) .
O16 C46 C49 109.35(19) .
C48 C46 C47 110.8(2) .
C48 C46 C49 109.7(2) .
C47 C46 C49 110.6(2) .
O14 C38 C39 106.20(18) .
O14 C38 C40 108.31(19) .
O14 C38 C41 111.96(18) .
C39 C38 C41 109.3(2) .
C40 C38 C39 110.4(2) .
C40 C38 C41 110.5(2) .
O2 C2 C4 107.02(18) .
O2 C2 C5 106.79(18) .
O2 C2 C3 111.33(18) .
C4 C2 C3 111.5(2) .
C5 C2 C4 110.5(2) .
C5 C2 C3 109.6(2) .
O4 C10 C11 106.77(19) .
O4 C10 C13 110.85(18) .
O4 C10 C12 107.97(19) .
C11 C10 C12 109.5(2) .
C13 C10 C11 111.3(2) .
C13 C10 C12 110.3(2) .
C100 C69 C82 113.4(2) .
C100 C100 C69 114.6(3) 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2 Cr2 3.0589(3) .
I2 C1 2.108(2) .
I1 Cr1 3.0433(3) .
I1 C1 2.165(2) .
Cr1 Si2 2.8555(6) .
Cr1 O9 1.9490(14) .
Cr1 O5 2.0580(14) .
Cr1 O6 2.2326(14) .
Cr1 O1 1.8691(14) .
Cr1 C1 2.046(2) .
Cr2 Si3 2.8137(6) .
Cr2 O9 2.1034(14) .
Cr2 O13 1.9356(14) .
Cr2 O5 2.0463(14) .
Cr2 O10 2.1376(14) .
Si2 O5 1.6174(14) .
Si2 O6 1.6643(15) .
Si2 O7 1.6074(15) .
Si2 O8 1.6150(15) .
Si1 O1 1.6005(15) .
Si1 O3 1.6332(15) .
Si1 O2 1.6244(16) .
Si1 O4 1.6210(17) .
Si4 O13 1.5820(15) .
Si4 O15 1.6326(15) .
Si4 O16 1.6409(16) .
Si4 O14 1.6432(16) .
Si3 O9 1.6155(15) .
Si3 O10 1.6711(15) .
Si3 O11 1.6043(16) .
Si3 O12 1.6110(16) .
O6 C14 1.474(2) .
O10 C26 1.484(2) .
O3 C6 1.438(2) .
O7 C18 1.453(2) .
O8 C22 1.450(2) .
O2 C2 1.444(2) .
O15 C42 1.437(3) .
O16 C46 1.438(3) .
O14 C38 1.447(3) .
O11 C30 1.452(2) .
O12 C34 1.446(3) .
O4 C10 1.435(3) .
C4 C2 1.519(3) .
C30 C32 1.515(4) .
C30 C33 1.513(4) .
C30 C31 1.508(3) .
C48 C46 1.517(3) .
C14 C16 1.514(3) .
C14 C17 1.519(3) .
C14 C15 1.507(3) .
C6 C7 1.522(3) .
C6 C9 1.523(3) .
C6 C8 1.522(3) .
C26 C29 1.525(3) .
C26 C27 1.515(3) .
C26 C28 1.516(3) .
C47 C46 1.528(4) .
C34 C35 1.524(3) .
C34 C36 1.520(3) .
C34 C37 1.522(3) .
C22 C25 1.516(3) .
C22 C24 1.517(3) .
C22 C23 1.520(3) .
C42 C43 1.522(3) .
C42 C45 1.529(3) .
C42 C44 1.519(3) .
C18 C19 1.519(3) .
C18 C21 1.512(3) .
C18 C20 1.522(3) .
C46 C49 1.529(3) .
C38 C39 1.521(3) .
C38 C40 1.520(3) .
C38 C41 1.523(3) .
C2 C5 1.516(3) .
C2 C3 1.525(3) .
C10 C11 1.525(3) .
C10 C13 1.520(3) .
C10 C12 1.528(3) .
C69 C82 1.521(5) .
C69 C100 1.515(4) .
C100 C100 1.513(6) 2_556
