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_7033516
_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 H37 Cl Ni P3 S2 +, C24 H20 B -, C4 H8 O'
_chemical_formula_sum            'C69 H65 B Cl Ni O P3 S2'
_chemical_formula_weight         1172.21
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-29
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-11-07 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                98.071(2)
_cell_angle_beta                 106.232(2)
_cell_angle_gamma                97.210(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8395(3)
_cell_length_b                   14.8535(4)
_cell_length_c                   15.4286(4)
_cell_measurement_reflns_used    29736
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.8400
_cell_measurement_theta_min      3.3350
_cell_volume                     2969.37(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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)
;
_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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      150.00(10)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details
;
  1 omega  -15.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000    0.0000 83

  2 omega  -21.00   39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   82.0000   84.0000 60

  3 omega  -51.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695    0.0000  150.0000 135

  4 omega  -19.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000 -150.0000 101

  5 omega  -54.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -68.0000   59.2969 98

  6 omega   -6.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -91.0000  -48.1336 57

  7 omega   -4.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -98.0000  142.5912 58

  8 omega   25.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -119.0000 -109.6485 41

  9 omega  -88.00   25.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -77.0000 -180.0000 113

 10 omega   -4.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000 -180.0000 56

 11 omega  -16.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   38.0000   60.0000 102

 12 omega  -63.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -57.0000  -90.0000 103

 13 omega   22.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695 -132.0000    8.7671 50

 14 omega  -65.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -38.0000    0.0000 102

 15 omega   -5.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -98.0000  142.5912 42

 16 omega   13.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -119.0000 -109.6485 53
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_12      -0.0320771000
_diffrn_orient_matrix_UB_13      -0.0388436000
_diffrn_orient_matrix_UB_21      0.0226971000
_diffrn_orient_matrix_UB_22      0.0362038000
_diffrn_orient_matrix_UB_23      -0.0172429000
_diffrn_orient_matrix_UB_31      0.0492161000
_diffrn_orient_matrix_UB_32      -0.0076539000
_diffrn_orient_matrix_UB_33      0.0238123000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            98379
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.431
_diffrn_reflns_theta_min         2.760
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       prism
_exptl_crystal_F_000             1228
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and hexane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         14473
_refine_ls_number_restraints     681
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0409P)^2^+2.3068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11298
_reflns_number_total             14473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03543g2.cif
_cod_data_source_block           rah140019
_cod_depositor_comments
'Adding full bibliography for 7033511--7033516.cif.'
_cod_original_cell_volume        2969.37(13)
_cod_database_code               7033516
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C60 H56 B1 P3 S2 Ni1'
_reflns_odcompleteness_completeness 99.86
_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. Uiso/Uaniso restraints and constraints
Uanis(C66A) = Uanis(C66B)
Uanis(C67A) = Uanis(C67B)
Uanis(C68A) = Uanis(C68B)
Uanis(C69B) = Uanis(C69A)
Uanis(O1A) = Uanis(O1B)
3. 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
4. Others
 Sof(O1B)=Sof(C66B)=Sof(H66C)=Sof(H66D)=Sof(C67B)=Sof(H67C)=Sof(H67D)=
 Sof(C68B)=Sof(H68C)=Sof(H68D)=Sof(C69B)=Sof(H69C)=Sof(H69D)=1-FVAR(1)
 Sof(O1A)=Sof(C66A)=Sof(H66A)=Sof(H66B)=Sof(C67A)=Sof(H67A)=Sof(H67B)=
 Sof(C68A)=Sof(H68A)=Sof(H68B)=Sof(C69A)=Sof(H69A)=Sof(H69B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C28(H28A,H28B), C29(H29A,H29B), C66A(H66A,
 H66B), C67A(H67A,H67B), C68A(H68A,H68B), C69A(H69A,H69B), C66B(H66C,H66D),
 C67B(H67C,H67D), C68B(H68C,H68D), C69B(H69C,H69D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62),
  C63(H63), C64(H64), C65(H65)
;
_shelx_res_checksum              67985
_shelx_hkl_checksum              39383
_olex2_submission_special_instructions 'No special instructions were received'