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_4088417
_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         'C16 H22 Ni3 S4, C H2 Cl2, B F4'
_chemical_formula_sum            'C17 H24 B Cl2 F4 Ni3 S4'
_chemical_formula_weight         690.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 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                 102.9697(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3664(5)
_cell_length_b                   12.7847(5)
_cell_length_c                   14.7048(6)
_cell_measurement_reflns_used    5421
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      2.135
_cell_volume                     2448.73(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      103.51
_diffrn_measured_fraction_theta_full 0.491
_diffrn_measured_fraction_theta_max 0.520
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.491
_diffrn_reflns_Laue_measured_fraction_max 0.520
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4501
_diffrn_reflns_point_group_measured_fraction_full 0.491
_diffrn_reflns_point_group_measured_fraction_max 0.520
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.463
_diffrn_reflns_theta_min         2.135
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.639377
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0630 before and 0.0489 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0740 before and 0.0588 after correction.
 The Ratio of minimum to maximum transmission is 0.86.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 53447 reflections, Rint = 0.0525
 (25439 with I > 3sig(I), Rint = 0.0382)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4501
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4033
_reflns_number_total             4501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           cm03n_0m
_cod_database_code               4088417
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.449
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.2681(11) 0.7319(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 F2A-B1A \\sim F2-B1 \\sim F3-B1 \\sim F3A-B1A \\sim F4A-B1A \\sim F4-B1 \\sim
F1-B1 \\sim F1A-B1A
 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
 F1A-F2A \\sim F1A-F3A \\sim F1A-F4A \\sim F2A-F3A \\sim F2A-F4A \\sim F3A-F4A
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F4 \\sim F3 \\sim F1A \\sim F4A \\sim F3A \\sim F2A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
B1 \\sim B1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 F1, F2, F4, F3, F1A, F4A, F3A, F2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B1A, B1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(B1A)=Sof(F1A)=Sof(F4A)=Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F4)=Sof(F3)=Sof(B1)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B), C6(H6A,H6B), C8(H8A,
 H8B), C101(H10C,H10D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C16(H16), C12(H12), C1(H1), C15(H15), C4(H4), C5(H5),
 C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'