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_4088408
_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         'C13 H16 Ni2 S2'
_chemical_formula_sum            'C13 H16 Ni2 S2'
_chemical_formula_weight         353.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                110.675(6)
_cell_angle_beta                 97.652(7)
_cell_angle_gamma                103.300(6)
_cell_formula_units_Z            4
_cell_length_a                   10.149(5)
_cell_length_b                   12.274(6)
_cell_length_c                   12.417(6)
_cell_measurement_reflns_used    977
_cell_measurement_temperature    181(2)
_cell_measurement_theta_max      24.42
_cell_measurement_theta_min      2.37
_cell_volume                     1368.7(12)
_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      181.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.895
_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  0.0764
_diffrn_reflns_av_unetI/netI     0.1392
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17061
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.227
_diffrn_reflns_theta_min         1.804
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.5795
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.1498 before and 0.0564 after correction. 
The Ratio of minimum to maximum transmission is 0.5804. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the 3 -3 2 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6062
_refine_ls_number_restraints     414
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0131P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3724
_reflns_number_total             6062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           bm23yas
_cod_depositor_comments
;

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C26 H32 Ni4 S4'
_cod_original_formula_weight         707.59
_cod_original_formula_moiety         '2(C13 H16 Ni2 S2)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1368.8(12)
_cod_database_code               4088408
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.368
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
2. Restrained distances 
 Ni2-C13A \\sim Ni2-C9 \\sim Ni2-C13 \\sim Ni2-C12A \\sim Ni2-C10 \\sim Ni2-C9A 
\\sim Ni2-C10A \\sim Ni2- 
 C11 \\sim Ni2-C12 \\sim Ni2-C11A 
 with sigma of 0.01 
 C9A-C13A \\sim C9-C10 \\sim C9-C13 \\sim C13A-C12A \\sim C12A-C11A \\sim 
C13-C12 \\sim C12-C11 \\sim C11A- 
 C10A \\sim C9A-C10A \\sim C11-C10 
 with sigma of 0.01 
3. Uiso/Uaniso restraints and constraints 
C17A \\sim C17 \\sim C16A \\sim C15 \\sim C15A \\sim C14A \\sim C18 \\sim C16 
\\sim C14 \\sim C18A: within 2A with sigma of 0.01 and sigma for terminal atoms 
of 0.02 
C10 \\sim C13 \\sim C11 \\sim C12 \\sim C12A \\sim C10A \\sim C9A \\sim C9 
\\sim C11A \\sim C13A: within 2A with sigma of 0.01 and sigma for terminal 
atoms of 0.02 
4. Others 
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C18A)=Sof(H18A)=Sof(C17A)= 
 Sof(H17A)=Sof(C16A)=Sof(H16A)=1-FVAR(1) 
 Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C17)=Sof(H17)= 
 Sof(C18)=Sof(H18)=FVAR(1) 
 Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)= 
 Sof(C13A)=Sof(H13A)=1-FVAR(2) 
 Sof(C13)=Sof(H13)=Sof(C12)=Sof(H12)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)= 
 Sof(C11)=Sof(H11)=FVAR(2) 
5.a Ternary CH refined with riding coordinates: 
 C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A) 
5.b Secondary CH2 refined with riding coordinates: 
 C19(H19A,H19B), C21(H21A,H21B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), 
 C20(H20A,H20B) 
5.c Aromatic/amide H refined with riding coordinates: 
 C26(H26), C25(H25), C22(H22), C1(H1), C23(H23), C13(H13), C5(H5), C16(H16), 
 C4(H4), C12(H12), C24(H24), C3(H3), C2(H2), C9(H9), C15(H15), C10(H10), 
 C14(H14), C17(H17), C18(H18), C11(H11), C14A(H14A), C15A(H15A), C18A(H18A), 
 C17A(H17A), C16A(H16A) 
;
_olex2_submission_special_instructions 'No special instructions were received'