#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/92/4309237.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_4309237
loop_
_publ_author_name
'Victor Wee Lin Ng'
'Seah Ling Kuan'
'Weng Kee Leong'
'Lip Lin Koh'
'Geok Kheng Tan'
'Lai Yoong Goh'
'Richard D. Webster'
_publ_section_title
;
Heterocyclic Thionates as a New Class of Bridging Ligands in Oxo-Centered
Triangular Cyclopentadienylchromium(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5229
_journal_page_last               5240
_journal_paper_doi               10.1021/ic048287e
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C35 H36 B Cr3 F4 N2 O3.5 S4'
_chemical_formula_weight         911.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.851(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3429(9)
_cell_length_b                   11.3164(6)
_cell_length_c                   18.6615(9)
_cell_measurement_reflns_used    2324
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.71
_cell_measurement_theta_min      2.24
_cell_volume                     3776.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14493
_diffrn_reflns_theta_full        29.43
_diffrn_reflns_theta_max         29.43
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.129
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.6867
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4989
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0635P)²+7.0463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                3782
_reflns_number_total             4989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048287esi20050415_071032_1.cif
_cod_data_source_block           sl1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C35 H36 B Cr3 F4 N2 O3.50 S4'
_cod_database_code               4309237
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.82764(4) 0.5000 0.20272(5) 0.0317(2) Uani 1 2 d S . .
Cr2 Cr 0.65572(3) 0.62896(6) 0.15628(3) 0.02793(17) Uani 1 1 d . . .
S1 S 0.82588(5) 0.65893(10) 0.28594(6) 0.0426(3) Uani 1 1 d . . .
S2 S 0.74243(6) 0.66751(12) 0.40444(6) 0.0457(3) Uani 1 1 d . . .
N1 N 0.67407(16) 0.6479(3) 0.26900(16) 0.0287(7) Uani 1 1 d . . .
O1 O 0.72420(18) 0.5000 0.16316(19) 0.0293(8) Uani 1 2 d S . .
O2 O 0.58574(19) 0.5000 0.1567(2) 0.0320(8) Uani 1 2 d SD . .
H2 H 0.5439(17) 0.5000 0.132(3) 0.050 Uiso 1 2 d SD . .
C1 C 0.7416(2) 0.6546(3) 0.3117(2) 0.0302(8) Uani 1 1 d . . .
C2 C 0.6184(2) 0.6548(3) 0.3091(2) 0.0305(8) Uani 1 1 d . . .
C3 C 0.5416(2) 0.6529(4) 0.2806(2) 0.0355(9) Uani 1 1 d . . .
H3 H 0.5225 0.6461 0.2297 0.043 Uiso 1 1 calc R . .
C4 C 0.4942(3) 0.6610(4) 0.3276(3) 0.0486(11) Uani 1 1 d . . .
H4 H 0.4422 0.6596 0.3087 0.058 Uiso 1 1 calc R . .
C5 C 0.5219(3) 0.6712(6) 0.4027(3) 0.0698(17) Uani 1 1 d . . .
H5 H 0.4883 0.6749 0.4340 0.084 Uiso 1 1 calc R . .
C6 C 0.5969(3) 0.6759(6) 0.4321(3) 0.0679(16) Uani 1 1 d . . .
H6 H 0.6152 0.6850 0.4830 0.081 Uiso 1 1 calc R . .
C7 C 0.6458(2) 0.6671(4) 0.3849(2) 0.0410(10) Uani 1 1 d . . .
C11 C 0.6055(3) 0.6972(4) 0.0449(2) 0.0459(11) Uani 1 1 d . . .
H11 H 0.5769 0.6487 0.0083 0.055 Uiso 1 1 calc R . .
C12 C 0.5779(3) 0.7652(4) 0.0957(2) 0.0480(11) Uani 1 1 d . . .
H12 H 0.5277 0.7708 0.0992 0.058 Uiso 1 1 calc R . .
C13 C 0.6385(3) 0.8231(5) 0.1401(3) 0.0572(13) Uani 1 1 d . . .
H13 H 0.6362 0.8749 0.1789 0.069 Uiso 1 1 calc R . .
C14 C 0.7035(3) 0.7906(5) 0.1167(3) 0.0576(14) Uani 1 1 d . . .
H14 H 0.7524 0.8163 0.1371 0.069 Uiso 1 1 calc R . .
C15 C 0.6819(3) 0.7137(5) 0.0579(3) 0.0535(13) Uani 1 1 d . . .
H15 H 0.7140 0.6786 0.0313 0.064 Uiso 1 1 calc R . .
C21 C 0.8615(4) 0.5000 0.0938(4) 0.065(2) Uani 1 2 d S . .
H21 H 0.8271 0.5000 0.0482 0.078 Uiso 1 2 calc SR . .
C22 C 0.8917(3) 0.5988(5) 0.1337(3) 0.0626(15) Uani 1 1 d . . .
H22 H 0.8800 0.6778 0.1203 0.075 Uiso 1 1 calc R . .
C23 C 0.9425(2) 0.5612(5) 0.1973(3) 0.0566(13) Uani 1 1 d . . .
H23 H 0.9713 0.6102 0.2334 0.068 Uiso 1 1 calc R . .
B1 B 0.3801(4) 0.5000 0.1170(4) 0.0412(16) Uani 1 2 d S . .
F1 F 0.31622(19) 0.5000 0.0622(2) 0.0585(11) Uani 1 2 d S . .
F2 F 0.4423(2) 0.5000 0.0848(2) 0.0819(16) Uani 1 2 d S . .
F3 F 0.3844(2) 0.4022(4) 0.1575(2) 0.1098(15) Uani 1 1 d . . .
O101 O 0.1944(5) 0.5000 0.2850(4) 0.147(4) Uani 1 2 d S . .
C102 C 0.2688(6) 0.5000 0.2965(5) 0.083(3) Uani 1 2 d S . .
H10A H 0.2853 0.5701 0.2737 0.099 Uiso 0.50 1 calc PR . .
H10B H 0.2853 0.4299 0.2737 0.099 Uiso 0.50 1 calc PR . .
C103 C 0.3024(7) 0.5000 0.3749(5) 0.097(3) Uani 1 2 d S . .
H10C H 0.3333 0.5705 0.3888 0.116 Uiso 0.50 1 calc PR . .
H10D H 0.3333 0.4295 0.3888 0.116 Uiso 0.50 1 calc PR . .
C104 C 0.2350(7) 0.5000 0.4111(4) 0.099(4) Uani 1 2 d S . .
H10E H 0.2348 0.4294 0.4415 0.119 Uiso 0.50 1 calc PR . .
H10F H 0.2348 0.5706 0.4415 0.119 Uiso 0.50 1 calc PR . .
C105 C 0.1696(6) 0.5000 0.3462(5) 0.084(3) Uani 1 2 d S . .
H10G H 0.1387 0.4298 0.3478 0.101 Uiso 0.50 1 calc PR . .
H10H H 0.1387 0.5702 0.3478 0.101 Uiso 0.50 1 calc PR . .
O201 O 0.4365(9) -0.022(3) 0.4594(9) 0.091(6) Uiso 0.25 1 d PD A -1
C202 C 0.4410(13) -0.034(3) 0.5322(13) 0.087(4) Uiso 0.25 1 d PD A -1
H20A H 0.4192 -0.1093 0.5428 0.104 Uiso 0.25 1 calc PR A -1
H20B H 0.4151 0.0307 0.5509 0.104 Uiso 0.25 1 calc PR A -1
C203 C 0.5164(13) -0.031(4) 0.5625(16) 0.087(4) Uiso 0.25 1 d PD A -1
H20C H 0.5308 -0.0989 0.5952 0.104 Uiso 0.25 1 calc PR A -1
H20D H 0.5292 0.0415 0.5913 0.104 Uiso 0.25 1 calc PR A -1
C204 C 0.5592(14) -0.035(3) 0.4980(16) 0.087(4) Uiso 0.25 1 d PD A -1
H20E H 0.5994 0.0238 0.5054 0.104 Uiso 0.25 1 calc PR A -1
H20F H 0.5804 -0.1135 0.4939 0.104 Uiso 0.25 1 calc PR A -1
C205 C 0.5041(12) -0.009(9) 0.4360(14) 0.087(4) Uiso 0.25 1 d PD A -1
H20G H 0.5062 -0.0634 0.3958 0.104 Uiso 0.25 1 calc PR A -1
H20H H 0.5097 0.0723 0.4193 0.104 Uiso 0.25 1 calc PR A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
O1 Cr1 C22 112.92(18) . 6_565 ?
O1 Cr1 C22 112.92(18) . . ?
C22 Cr1 C22 60.3(3) 6_565 . ?
O1 Cr1 C23 149.37(17) . 6_565 ?
C22 Cr1 C23 36.59(19) 6_565 6_565 ?
C22 Cr1 C23 60.50(19) . 6_565 ?
O1 Cr1 C23 149.37(17) . . ?
C22 Cr1 C23 60.50(19) 6_565 . ?
C22 Cr1 C23 36.59(19) . . ?
C23 Cr1 C23 36.0(3) 6_565 . ?
O1 Cr1 C21 95.9(2) . . ?
C22 Cr1 C21 36.09(18) 6_565 . ?
C22 Cr1 C21 36.09(18) . . ?
C23 Cr1 C21 60.6(2) 6_565 . ?
C23 Cr1 C21 60.6(2) . . ?
O1 Cr1 S1 95.59(8) . . ?
C22 Cr1 S1 147.32(14) 6_565 . ?
C22 Cr1 S1 94.77(16) . . ?
C23 Cr1 S1 114.34(15) 6_565 . ?
C23 Cr1 S1 86.85(13) . . ?
C21 Cr1 S1 129.39(5) . . ?
O1 Cr1 S1 95.59(8) . 6_565 ?
C22 Cr1 S1 94.77(16) 6_565 6_565 ?
C22 Cr1 S1 147.32(14) . 6_565 ?
C23 Cr1 S1 86.85(13) 6_565 6_565 ?
C23 Cr1 S1 114.34(15) . 6_565 ?
C21 Cr1 S1 129.39(5) . 6_565 ?
S1 Cr1 S1 98.10(7) . 6_565 ?
O1 Cr2 O2 81.44(11) . . ?
O1 Cr2 N1 93.17(14) . . ?
O2 Cr2 N1 91.84(14) . . ?
O1 Cr2 C15 97.24(16) . . ?
O2 Cr2 C15 126.36(19) . . ?
N1 Cr2 C15 141.43(18) . . ?
O1 Cr2 C11 117.34(16) . . ?
O2 Cr2 C11 97.37(17) . . ?
N1 Cr2 C11 149.07(16) . . ?
C15 Cr2 C11 36.30(17) . . ?
O1 Cr2 C14 110.42(17) . . ?
O2 Cr2 C14 158.06(17) . . ?
N1 Cr2 C14 105.40(18) . . ?
C15 Cr2 C14 36.40(19) . . ?
C11 Cr2 C14 60.94(18) . . ?
O1 Cr2 C12 154.00(16) . . ?
O2 Cr2 C12 99.93(16) . . ?
N1 Cr2 C12 112.66(15) . . ?
C15 Cr2 C12 60.84(17) . . ?
C11 Cr2 C12 36.67(17) . . ?
C14 Cr2 C12 61.17(18) . . ?
O1 Cr2 C13 146.37(17) . . ?
O2 Cr2 C13 131.74(17) . . ?
N1 Cr2 C13 91.24(16) . . ?
C15 Cr2 C13 60.8(2) . . ?
C11 Cr2 C13 60.83(18) . . ?
C14 Cr2 C13 36.8(2) . . ?
C12 Cr2 C13 36.37(18) . . ?
O1 Cr2 Cr2 40.21(8) . 6_565 ?
O2 Cr2 Cr2 41.37(8) . 6_565 ?
N1 Cr2 Cr2 95.97(9) . 6_565 ?
C15 Cr2 Cr2 115.65(15) . 6_565 ?
C11 Cr2 Cr2 110.41(13) . 6_565 ?
C14 Cr2 Cr2 145.34(16) . 6_565 ?
C12 Cr2 Cr2 133.74(14) . 6_565 ?
C13 Cr2 Cr2 170.03(14) . 6_565 ?
C1 S1 Cr1 107.73(13) . . ?
C7 S2 C1 90.48(19) . . ?
C1 N1 C2 111.9(3) . . ?
C1 N1 Cr2 122.7(2) . . ?
C2 N1 Cr2 125.4(2) . . ?
Cr1 O1 Cr2 128.19(9) . 6_565 ?
Cr1 O1 Cr2 128.19(9) . . ?
Cr2 O1 Cr2 99.57(15) 6_565 . ?
Cr2 O2 Cr2 97.25(15) 6_565 . ?
N1 C1 S1 128.0(3) . . ?
N1 C1 S2 114.0(3) . . ?
S1 C1 S2 117.9(2) . . ?
C3 C2 N1 126.4(3) . . ?
C3 C2 C7 119.6(3) . . ?
N1 C2 C7 114.1(3) . . ?
C4 C3 C2 119.2(4) . . ?
C3 C4 C5 120.7(4) . . ?
C6 C5 C4 121.4(4) . . ?
C5 C6 C7 118.4(5) . . ?
C6 C7 C2 120.7(4) . . ?
C6 C7 S2 129.8(4) . . ?
C2 C7 S2 109.5(3) . . ?
C15 C11 C12 108.2(4) . . ?
C15 C11 Cr2 71.8(2) . . ?
C12 C11 Cr2 72.2(2) . . ?
C13 C12 C11 107.5(4) . . ?
C13 C12 Cr2 71.8(3) . . ?
C11 C12 Cr2 71.1(2) . . ?
C12 C13 C14 108.1(5) . . ?
C12 C13 Cr2 71.8(3) . . ?
C14 C13 Cr2 71.3(3) . . ?
C15 C14 C13 107.2(4) . . ?
C15 C14 Cr2 71.5(3) . . ?
C13 C14 Cr2 71.8(3) . . ?
C11 C15 C14 108.9(4) . . ?
C11 C15 Cr2 71.9(2) . . ?
C14 C15 Cr2 72.1(3) . . ?
C22 C21 C22 107.4(7) 6_565 . ?
C22 C21 Cr1 70.9(3) 6_565 . ?
C22 C21 Cr1 70.9(3) . . ?
C21 C22 C23 108.6(5) . . ?
C21 C22 Cr1 73.0(3) . . ?
C23 C22 Cr1 72.2(3) . . ?
C23 C23 C22 107.7(3) 6_565 . ?
C23 C23 Cr1 71.99(14) 6_565 . ?
C22 C23 Cr1 71.2(2) . . ?
F3 B1 F3 112.4(7) . 6_565 ?
F3 B1 F1 110.8(4) . . ?
F3 B1 F1 110.8(4) 6_565 . ?
F3 B1 F2 107.0(4) . . ?
F3 B1 F2 107.0(4) 6_565 . ?
F1 B1 F2 108.8(5) . . ?
C105 O101 C102 113.5(8) . . ?
O101 C102 C103 110.6(9) . . ?
C102 C103 C104 103.9(9) . . ?
C105 C104 C103 102.8(7) . . ?
O101 C105 C104 109.3(9) . . ?
C202 O201 C205 117.5(18) . . ?
O201 C202 C203 104(2) . . ?
C202 C203 C204 108(2) . . ?
C205 C204 C203 103.7(17) . . ?
C204 C205 O201 104(2) . . ?
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
Cr1 O1 1.877(3) . ?
Cr1 C22 2.228(4) 6_565 ?
Cr1 C22 2.228(4) . ?
Cr1 C23 2.241(4) 6_565 ?
Cr1 C23 2.241(4) . ?
Cr1 C21 2.254(7) . ?
Cr1 S1 2.3811(12) . ?
Cr1 S1 2.3811(12) 6_565 ?
Cr2 O1 1.911(2) . ?
Cr2 O2 1.945(2) . ?
Cr2 N1 2.066(3) . ?
Cr2 C15 2.216(4) . ?
Cr2 C11 2.216(4) . ?
Cr2 C14 2.224(5) . ?
Cr2 C12 2.230(4) . ?
Cr2 C13 2.231(5) . ?
Cr2 Cr2 2.9187(13) 6_565 ?
S1 C1 1.719(4) . ?
S2 C7 1.729(4) . ?
S2 C1 1.734(4) . ?
N1 C1 1.318(5) . ?
N1 C2 1.396(4) . ?
O1 Cr2 1.911(2) 6_565 ?
O2 Cr2 1.945(2) 6_565 ?
C2 C3 1.391(5) . ?
C2 C7 1.398(6) . ?
C3 C4 1.369(6) . ?
C4 C5 1.385(7) . ?
C5 C6 1.365(7) . ?
C6 C7 1.393(6) . ?
C11 C15 1.381(6) . ?
C11 C12 1.399(6) . ?
C12 C13 1.392(7) . ?
C13 C14 1.407(7) . ?
C14 C15 1.387(7) . ?
C21 C22 1.388(7) 6_565 ?
C21 C22 1.388(7) . ?
C22 C23 1.403(7) . ?
C23 C23 1.386(11) 6_565 ?
B1 F3 1.331(5) . ?
B1 F3 1.331(5) 6_565 ?
B1 F1 1.373(8) . ?
B1 F2 1.403(8) . ?
O101 C105 1.319(11) . ?
O101 C102 1.333(11) . ?
C102 C103 1.454(12) . ?
C103 C104 1.536(15) . ?
C104 C105 1.503(14) . ?
O201 C202 1.35(2) . ?
O201 C205 1.41(2) . ?
C202 C203 1.37(2) . ?
C203 C204 1.58(3) . ?
C204 C205 1.39(2) . ?
