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_4088412
_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         'C12 H14 Ni2 S2, B F4'
_chemical_formula_sum            'C12 H14 B F4 Ni2 S2'
_chemical_formula_weight         426.58
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-09
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_audit_update_record
;
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.854(3)
_cell_length_b                   10.221(3)
_cell_length_c                   11.434(3)
_cell_measurement_reflns_used    3640
_cell_measurement_temperature    183.15
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.38
_cell_volume                     1502.2(7)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      183.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens Platform/CCD'
_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_radiation_wavelength_id  fm02v_0m
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11276
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.813
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.5109
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1853 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.5117.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             860
_exptl_crystal_id                fm02v_0m
_exptl_crystal_preparation
;
The data crystal was mounted using oil (Parantone-N) to a 
0.3 mm cryo-loop (Hampton Research) with the 0 0 1 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.671
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.2728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                1265
_reflns_number_total             1441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           fm02v_0m
_cod_database_code               4088412
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H1 of C1, H2 of C2, H3 of C3, H4 of C4, H5 of C5, {H6B,H6A} of C6, {H7A,
  H7B} of C7
2. Others
 Fixed Sof: F4(0.5) H6B(0.5) H6A(0.5) H7A(0.5) H7B(0.5) B1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6B,H6A), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5)
;