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_4088410
_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         'C22 H18 Ni3 S4'
_chemical_formula_sum            'C22 H18 Ni3 S4'
_chemical_formula_weight         586.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-26
_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            4
_cell_length_a                   7.73480(10)
_cell_length_b                   15.8097(3)
_cell_length_c                   17.5647(3)
_cell_measurement_reflns_used    5343
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.608
_cell_measurement_theta_min      2.576
_cell_volume                     2147.90(6)
_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      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18300
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.789
_diffrn_reflns_theta_min         1.733
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.999
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9152
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0709 before and 0.0645 after correction. 
The Ratio of minimum to maximum transmission is 0.9166. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1192
_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 -2 face roughly
parallel to the spindle axis.
;
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
; 
 Flack x determined using 1566 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0086P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4210
_reflns_number_total             5076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           cm50e_0m
_cod_database_code               4088410
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.473
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
2. Uiso/Uaniso restraints and constraints 
C21A \\sim C21 \\sim C20A \\sim C20 \\sim C19A \\sim C19 \\sim C18A \\sim C18 
\\sim C22A \\sim C22: within 1.7A with sigma of 0.01 and sigma for terminal 
atoms of 0.02 
C5A \\sim C5 \\sim C4A \\sim C4 \\sim C3A \\sim C3 \\sim C2A \\sim C2 \\sim C1A 
\\sim C1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 
3. Others 
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C1A)=Sof(H1A)= 
 Sof(C2A)=Sof(H2A)=1-FVAR(1) 
 Sof(C5)=Sof(H5)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=Sof(C2)=Sof(H2)=Sof(C1)= 
 Sof(H1)=FVAR(1) 
 Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C18A)=Sof(H18A)=Sof(C19A)= 
 Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(2) 
 Sof(C22)=Sof(H22)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)= 
 Sof(C21)=Sof(H21)=FVAR(2) 
4.a Aromatic/amide H refined with riding coordinates: 
C3A(H3A), C4A(H4A), C5A(H5A), C1A(H1A), C2A(H2A), C5(H5), C4(H4), C3(H3), 
C2(H2), C1(H1), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
C16(H16), C21A(H21A), C22A(H22A), C18A(H18A), C19A(H19A), C20A(H20A), 
C22(H22), C18(H18), C19(H19), C20(H20), C21(H21) 
4.b Fitted pentagon refined as free rotating group: 
C3A(C4A,C5A,C1A,C2A), C5(C4,C3,C2,C1), C21A(C22A,C18A,C19A,C20A), C22(C18,C19,
C20,C21) 
;
_olex2_submission_special_instructions 'No special instructions were received'