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_4088409
_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         'C16 H22 Ni3 S4'
_chemical_formula_sum            'C16 H22 Ni3 S4'
_chemical_formula_weight         518.70
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-28
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.3769(4)
_cell_length_b                   13.3769(4)
_cell_length_c                   25.1645(9)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.524
_cell_measurement_theta_min      2.694
_cell_volume                     4503.0(2)
_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      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.576
_diffrn_reflns_theta_min         2.694
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.849
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.1558 before and 0.0730 after correction. 
The Ratio of minimum to maximum transmission is 0.7298. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_description       Square
_exptl_crystal_F_000             2128
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the 2 -2 1 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.65(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0249
_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/[\s^2^(Fo^2^)+(0.0265P)^2^+4.4948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3089
_reflns_number_total             3456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           mo_cd09r
_cod_original_cell_volume        4503.0(3)
_cod_database_code               4088409
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.374
_olex2_refinement_description
; 
1. Twinned data refinement 
 Scales: 0.35(2) 0.65(2) 
2. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
3.a Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C5(H5A,H5B), C2(H2A,H2B) 
3.b Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C9(H9), C10(H10), C16(H16) 
;
_shelx_fab_checksum              6526
_olex2_submission_special_instructions 'No special instructions were received'