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_4088407
_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         'C14 H18 Ni3 S4'
_chemical_formula_sum            'C14 H18 Ni3 S4'
_chemical_formula_weight         490.65
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-29
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 93.189(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7434(13)
_cell_length_b                   11.8704(15)
_cell_length_c                   25.984(3)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.245
_cell_measurement_theta_min      2.325
_cell_volume                     3308.6(7)
_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  0.0661
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            110087
_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         27.292
_diffrn_reflns_theta_min         1.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.871
_exptl_absorpt_correction_T_max  0.5222
_exptl_absorpt_correction_T_min  0.2114
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.1353 before and 0.0860 after correction. 
The Ratio of minimum to maximum transmission is 0.4048. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description       prism
_exptl_crystal_F_000             2000
_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 -3 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.629
_exptl_crystal_size_mid          0.433
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+1.9376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6589
_reflns_number_total             7433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           c13k_0m
_cod_database_code               4088407
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.517
_shelx_estimated_absorpt_t_min   0.194
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
2. Uiso/Uaniso restraints and constraints 
C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C3A \\sim C4 \\sim C4A \\sim C5 
\\sim C5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 
3. Others 
 Sof(C1A)=Sof(H1A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)= 
 Sof(C2A)=Sof(H2A)=1-FVAR(1) 
 Sof(C1)=Sof(H1)=Sof(C5)=Sof(H5)=Sof(C2)=Sof(H2)=Sof(C4)=Sof(H4)=Sof(C3)= 
 Sof(H3)=FVAR(1) 
4.a Secondary CH2 refined with riding coordinates: 
 C9(H9A,H9B), C8(H8A,H8B), C6(H6A,H6B), C20(H20A,H20B), C22(H22A,H22B), 
 C23(H23A,H23B), C21(H21A,H21B), C7(H7A,H7B) 
4.b Aromatic/amide H refined with riding coordinates: 
 C12(H12), C10(H10), C13(H13), C11(H11), C14(H14), C25(H25), C24(H24), 
 C18(H18), C26(H26), C19(H19), C17(H17), C28(H28), C16(H16), C27(H27), C15(H15), 
  C1(H1), C5(H5), C2(H2), C4(H4), C3(H3), C1A(H1A), C5A(H5A), C4A(H4A), 
 C3A(H3A), C2A(H2A) 
;
_olex2_submission_special_instructions 'No special instructions were received'