Mechanisms and rates of proton transfer to coordinated carboxydithioates: studies on [Ni(S2CR){PhP(CH2CH2PPh2)2}](+) (R = Me, Et, Bu(n) or Ph).
Alwaaly, Ahmed; Clegg, William; Henderson, Richard A.; Probert, Michael R.; Waddell, Paul G.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 3307–3317; doi:10.1039/c4dt03543g

data_7033512
_publ_section_title
;
 Mechanisms and rates of proton transfer to coordinated carboxydithioates:
 studies on [Ni(S2CR){PhP(CH2CH2PPh2)2}](+) (R = Me, Et, Bu(n) or Ph).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3307
_journal_page_last               3317
_journal_paper_doi               10.1039/c4dt03543g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C41 H38 Ni P3 S2 +, C24 H20 B -, C4 H8 O'
_chemical_formula_sum            'C69 H66 B Ni O P3 S2'
_chemical_formula_weight         1137.76
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-13
_audit_creation_method
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Olex2 1.2-alpha
(compiled 2014.05.21 svn.r2942 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2014-11-07 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.8301(16)
_cell_length_b                   16.6153(5)
_cell_length_c                   18.1236(5)
_cell_measurement_reflns_used    12293
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.7390
_cell_measurement_theta_min      3.6180
_cell_volume                     11692.9(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -79.00  -52.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.9070  -57.0000   60.0000 27

  2 omega  -80.00  -38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.9070  -38.0000  -90.0000 42

  3 omega   -4.00   41.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000  120.0000 45

  4 omega  -16.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000   30.0000 35

  5 omega   -4.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000  -60.0000 43
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
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_diffrn_orient_matrix_UB_11      -0.0072112000
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_diffrn_orient_matrix_UB_13      -0.0321376000
_diffrn_orient_matrix_UB_21      -0.0131760000
_diffrn_orient_matrix_UB_22      0.0176802000
_diffrn_orient_matrix_UB_23      0.0217051000
_diffrn_orient_matrix_UB_31      0.0103870000
_diffrn_orient_matrix_UB_32      0.0346695000
_diffrn_orient_matrix_UB_33      0.0052435000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52089
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             4784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and hexane'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.518
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_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         11747
_refine_ls_number_restraints     642
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0209P)^2^+17.0726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9140
_reflns_number_total             11747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03543g2.cif
_cod_data_source_block           rah140012_fa
_cod_depositor_comments
'Adding full bibliography for 7033511--7033516.cif.'
_cod_database_code               7033512
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C69 H66 B1 O1 P3 S2 Ni1'
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C20(H20A,H20B), C21(H21A,H21B), C29(H29A,H29B), C2T(H2TA,
 H2TB), C1T(H1TA,H1TB), C3T(H3TA,H3TB), C4T(H4TA,H4TB)
3.b Aromatic/amide H refined with riding coordinates:
 C2B(H2B), C7(H7), C35(H35), C31(H31), C11(H11), C13(H13), C18B(H18B),
 C8B(H8B), C41(H41), C9(H9), C3(H3), C12B(H12B), C24B(H24B), C37(H37), C17(H17),
  C33(H33), C15B(H15B), C14B(H14B), C6B(H6B), C20B(H20C), C23(H23), C6(H6),
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 C22B(H22B), C5(H5), C10B(H10B), C4B(H4B), C11B(H11B), C23B(H23B), C40(H40),
 C18(H18), C24(H24), C39(H39), C16(H16), C25(H25), C38(H38), C26(H26)
;
_shelx_res_checksum              61878
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_olex2_submission_special_instructions 'No special instructions were received'