Effect of Pyramidalization of the M2(SR)2Center: The Case of (C5H5)2Ni2(SR)2
Chambers, Geoffrey M.; Rauchfuss, Thomas B.; Arrigoni, Federica; Zampella, Giuseppe; Organometallics 35 (2016) 836–; doi:10.1021/acs.organomet.6b00068

data_4088414
_publ_section_title
;
 Effect of Pyramidalization of the M2(SR)2Center: The Case of
 (C5H5)2Ni2(SR)2
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              836
_journal_paper_doi               10.1021/acs.organomet.6b00068
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         '2(C9 H18 Ni3 S6), C H Cl3'
_chemical_formula_sum            'C19 H37 Cl3 Ni6 S12'
_chemical_formula_weight         1108.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-31
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 108.5390(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9835(10)
_cell_length_b                   10.0573(5)
_cell_length_c                   18.4519(8)
_cell_measurement_reflns_used    9350
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      25.353
_cell_measurement_theta_min      2.292
_cell_volume                     3516.0(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      102.28
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            89920
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.486
_diffrn_reflns_theta_min         2.233
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.105
_exptl_absorpt_correction_T_max  0.8592
_exptl_absorpt_correction_T_min  0.7384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. 
wR2(int) was 0.0758 before and 0.0601 after correction. 
The Ratio of minimum to maximum transmission is 0.8594. 
The \l/2 correction factor is 0.00150. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the -1 0 0 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0180
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0310
_refine_ls_wR_factor_ref         0.0328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5210
_reflns_number_total             6491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           cd72lsa
_cod_database_code               4088414
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.659
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C014(H014) 
2.b Secondary CH2 refined with riding coordinates: 
 C00M(H00Q,H00R), C00N(H00A,H00B), C00O(H00S,H00T), C00P(H00U,H00V), C00Q(H00C, 
 H00D), C00R(H00E,H00F), C00S(H00G,H00H), C00T(H00W,H00X), C00U(H00Y,H), 
 C00V(H00I,H00J), C00W(H00K,H00L), C00X(H00M,H00N), C00Y(H00O,H00P), C00Z(H00Z, 
 HA), C010(H01C,H01D), C011(H01E,H01F), C012(H01A,H01B), C013(H01G,H01H) 
;
_olex2_submission_special_instructions 'No special instructions were received'