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_7033514
_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         'C42 H40 Ni P3 S2 +, C24 H20 B -, 1(C H Cl3)'
_chemical_formula_sum            'C67 H61 B Cl3 Ni P3 S2'
_chemical_formula_weight         1199.05
_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             2014-08-01
_audit_creation_method
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Olex2 1.2-alpha
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
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_audit_update_record
;
2014-11-07 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                93.5320(17)
_cell_angle_beta                 106.7120(17)
_cell_angle_gamma                98.1580(17)
_cell_formula_units_Z            2
_cell_length_a                   13.9329(3)
_cell_length_b                   14.4258(3)
_cell_length_c                   15.6129(3)
_cell_measurement_reflns_used    27385
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.8750
_cell_measurement_theta_min      3.0040
_cell_volume                     2957.72(11)
_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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -38.00   57.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   57.0000    0.0000 95

  2 omega  -38.00   65.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   57.0000  120.0000 103

  3 omega  -84.00    7.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -77.0000  150.0000 91

  4 omega  -88.00   20.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -77.0000    0.0000 108

  5 omega  -38.00   58.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289   57.0000  -90.0000 96

  6 omega   13.00   76.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   57.0000  -90.0000 63

  7 omega    8.00   53.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000  -96.0000  173.3762 45

  8 omega    5.00   56.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -102.0000  111.7775 51

  9 omega  -88.00   25.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -77.0000 -180.0000 113

 10 omega  -83.00   21.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.8289  -57.0000  -90.0000 104

 11 omega  -36.00   92.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695   19.0000  120.0000 128

 12 omega   -4.00   52.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000  -90.0000 56

 13 omega   -4.00   52.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       10.4695  -99.0000 -120.0000 56

 14 omega   -1.00   56.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -102.0000  111.7775 57

 15 omega    7.00   61.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0000 -111.0000   -8.7787 54
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0348573000
_diffrn_orient_matrix_UB_12      0.0006371000
_diffrn_orient_matrix_UB_13      -0.0431161000
_diffrn_orient_matrix_UB_21      -0.0107460000
_diffrn_orient_matrix_UB_22      -0.0499335000
_diffrn_orient_matrix_UB_23      -0.0050619000
_diffrn_orient_matrix_UB_31      -0.0396965000
_diffrn_orient_matrix_UB_32      0.0016275000
_diffrn_orient_matrix_UB_33      0.0197970000
_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     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            94253
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform and hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         13375
_refine_ls_number_restraints     694
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0346P)^2^+2.4840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10653
_reflns_number_total             13375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03543g2.cif
_cod_data_source_block           rah140020_fa
_cod_depositor_comments
'Adding full bibliography for 7033511--7033516.cif.'
_cod_database_code               7033514
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C66 H60 B1 P3 S2 Ni1'
_reflns_odcompleteness_completeness 99.85
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl1A) = Uanis(Cl1B) = Uanis(Cl1C)
Uanis(Cl2A) = Uanis(Cl2B) = Uanis(Cl2C)
Uanis(Cl3A) = Uanis(Cl3B) = Uanis(Cl3C)
Uanis(C67A) = Uanis(C67B) = Uanis(C67C)
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. Same fragment restrains
{Cl1C, Cl2C, Cl3C, C67C}
{Cl1A, Cl2A, Cl3A, C67A}
as
{Cl1B, Cl2B, Cl3B, C67B}
5. Others
 1*[Sof(Cl1A)+Sof(Cl2A)+Sof(Cl3A)+Sof(C67A)+Sof(H67A)]+1*[Sof(Cl1B)+Sof(Cl2B)+
 Sof(Cl3B)+Sof(C67B)+Sof(H67B)]+1*[Sof(Cl1C)+Sof(Cl2C)+Sof(Cl3C)+Sof(C67C)+
 Sof(H67C)]=1 with esd of 0.001
 Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(C67A)=Sof(H67A)=FVAR(1)
 Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(C67B)=Sof(H67B)=FVAR(2)
 Sof(Cl1C)=Sof(Cl2C)=Sof(Cl3C)=Sof(C67C)=Sof(H67C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C67A(H67A), C67B(H67B), C67C(H67C)
6.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C29(H29A,H29B), C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53),
 C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              93711
_shelx_hkl_checksum              39914
_olex2_submission_special_instructions 'No special instructions were received'