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_4088413
_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, B F4'
_chemical_formula_sum            'C13 H16 B F4 Ni2 S2'
_chemical_formula_weight         440.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5362(5)
_cell_length_b                   10.0545(4)
_cell_length_c                   11.4337(5)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.392
_cell_measurement_theta_min      2.332
_cell_volume                     1556.12(11)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_min         2.332
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8580
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.1451 before and 0.0485 after correction. 
The Ratio of minimum to maximum transmission is 0.8580. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_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 3 -4 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0189P)^2^+1.6882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1539
_reflns_number_total             1697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           mo_cd63n_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Integration' was
changed to 'integration' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088413
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.507
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
2. Restrained distances 
 S2-C2 \\sim S1-C3 
 with sigma of 0.01 
 C4-C2 \\sim C4-C3 
 with sigma of 0.01 
 F4-B1 \\sim F3-B1 \\sim F2-B1 \\sim F1-B1 
 with sigma of 0.01 
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4 
 with sigma of 0.01 
3. Uiso/Uaniso restraints and constraints 
C2 \\sim C4 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms 
of 0.02 
F3 \\sim F2 \\sim F1 \\sim F4 \\sim B1: within 2A with sigma of 0.01 and sigma 
for terminal atoms of 0.02 
4. Rigid body (RIGU) restrains 
 F2, F4, B1, F3, F1 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
5. Others 
 Fixed Sof: F4(0.5) F2(0.5) F3(0.5) F1(0.5) B1(0.5) C2(0.5) H2A(0.5) H2B(0.5) 
 C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) 
6.a Secondary CH2 refined with riding coordinates: 
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B) 
6.b Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C11(H11), C6(H6), C1(H1) 
;
_olex2_submission_special_instructions 'No special instructions were received'