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_4088418
_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         '2(C7 H10 Ni S)'
_chemical_formula_sum            'C14 H20 Ni2 S2'
_chemical_formula_weight         369.84
_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     direct
_audit_creation_date             2015-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                88.053(11)
_cell_angle_beta                 69.956(9)
_cell_angle_gamma                88.644(10)
_cell_formula_units_Z            2
_cell_length_a                   8.106(2)
_cell_length_b                   9.644(3)
_cell_length_c                   10.354(3)
_cell_measurement_reflns_used    4834
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      27.145
_cell_measurement_theta_min      2.782
_cell_volume                     759.9(4)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      102.28
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3340
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.106
_diffrn_reflns_theta_min         2.776
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.492187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1072 before and 0.0401 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 0.1011 before and 0.0407 after correction.
 The Ratio of minimum to maximum transmission is 0.66.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 42076 reflections, Rint = 0.0332
 (31918 with I > 3sig(I), Rint = 0.0286)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     418
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0172P)^2^+1.5401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3142
_reflns_number_total             3340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00068_si_002.cif
_cod_data_source_block           cd89lt4
_cod_database_code               4088418
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5206(13) 0.4794(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S1-C6 \\sim S1A-C6A
 with sigma of 0.02
 C7A-C6A \\sim C7-C6
 with sigma of 0.02
 C14A-C13A \\sim C14-C13
 with sigma of 0.02
 S2-C13 \\sim S2A-C13A
 with sigma of 0.02
 C7-C6 \\sim C7A-C6A \\sim C14A-C13A \\sim C14-C13
 with sigma of 0.01
 Ni1-S1 \\sim Ni1-S1A \\sim Ni2-S2 \\sim Ni2-S2A
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C7 \\sim C7A \\sim C6 \\sim C6A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C10A \\sim C10 \\sim C9 \\sim C8 \\sim C12 \\sim C11 \\sim C9A \\sim C8A \\sim
C12A \\sim C11A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C13 \\sim C14 \\sim C14A \\sim C13A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C4 \\sim C5A \\sim C1 \\sim C1A \\sim C5 \\sim C2A \\sim C2 \\sim C3A \\sim C3
\\sim C4A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C14A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(S2) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(S2A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 S2, S1, S1A, S2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(S1A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 1-FVAR(1)
 Sof(S1)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
 Sof(C5A)=Sof(H5A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=
 Sof(C4A)=Sof(H4A)=1-FVAR(2)
 Sof(C3)=Sof(H3)=Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=Sof(C5)=Sof(H5)=Sof(C4)=
 Sof(H4)=FVAR(2)
 Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(H8A)=Sof(C12A)=Sof(H12A)=
 Sof(C11A)=Sof(H11A)=1-FVAR(3)
 Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(H8)=Sof(C12)=
 Sof(H12)=FVAR(3)
 Sof(S2A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=1-FVAR(4)
 Sof(S2)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C6(H6A,H6B), C6A(H6AA,H6AB), C13A(H13C,H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C1(H1), C5(H5), C4(H4), C11(H11), C10(H10), C9(H9), C8(H8),
 C12(H12), C5A(H5A), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C10A(H10A),
 C9A(H9A), C8A(H8A), C12A(H12A), C11A(H11A)
7.c Fitted pentagon refined as free rotating group:
 C3(C2,C1,C5,C4), C11(C10,C9,C8,C12), C5A(C1A,C2A,C3A,C4A), C10A(C9A,C8A,C12A,
 C11A)
7.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C14A(H14D,H14E,H14F)
;
_olex2_submission_special_instructions 'No special instructions were received'