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_7033515
_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 O P3 S2 +, C24 H20 B -, C4 H8 O'
_chemical_formula_sum            'C70 H68 B Ni O2 P3 S2'
_chemical_formula_weight         1167.79
_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             2013-08-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.07.19 svn.r2750, GUI svn.r4539)
;
_audit_update_record
;
2014-11-07 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                93.2523(19)
_cell_angle_beta                 106.7604(19)
_cell_angle_gamma                98.3313(19)
_cell_formula_units_Z            2
_cell_length_a                   13.9067(9)
_cell_length_b                   14.4762(9)
_cell_length_c                   15.5552(10)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.28
_cell_volume                     2950.8(3)
_computing_cell_refinement       'Apex2 - SAINT (Bruker 2013)'
_computing_data_collection       'Apex2 (Bruker 2013)'
_computing_data_reduction        'Apex2 - SAINT (Bruker 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'Bruker Photon 100 Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_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            40258
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         2.084
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0998 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.8810.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and hexane'
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         13545
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0553P)^2^+1.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10330
_reflns_number_total             13545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03543g2.cif
_cod_data_source_block           rah130008
_cod_depositor_comments
'Adding full bibliography for 7033511--7033516.cif.'
_cod_database_code               7033515
_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. Restrained distances
 C7T-C6T \\sim C2T-C3T
 with sigma of 0.02
 C4T-C3T \\sim C7T-C8T \\sim C2T-C1T \\sim C6T-C5T
 with sigma of 0.02
 O2T-C8T \\sim O1T-C4T \\sim O1T-C1T \\sim O2T-C5T
 with sigma of 0.02
 C7T-C5T \\sim C3T-C1T \\sim C6T-C4T \\sim C8T-C2T
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2T \\sim C8T \\sim C7T \\sim C6T \\sim C5T \\sim C2T \\sim C3T \\sim C4T \\sim
C1T \\sim O1T: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C8T) = Uanis(C4T)
Uanis(C7T) = Uanis(C3T)
Uanis(C6T) = Uanis(C2T)
Uanis(C5T) = Uanis(C1T)
Uanis(O2T) = Uanis(O1T)
4. Others
 Fixed Sof: O1T(0.4) O2T(0.6) C1T(0.4) H1TA(0.4) H1TB(0.4) C2T(0.4) H2TA(0.4)
 H2TB(0.4) C3T(0.4) H3TA(0.4) H3TB(0.4) C4T(0.4) H4TA(0.4) H4TB(0.4) C5T(0.6)
 H5TA(0.6) H5TB(0.6) C6T(0.6) H6TA(0.6) H6TB(0.6) C7T(0.6) H7TA(0.6) H7TB(0.6)
 C8T(0.6) H8TA(0.6) H8TB(0.6)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C29(H29A,H29B), C30(H30A,H30B), C1T(H1TA,
 H1TB), C2T(H2TA,H2TB), C3T(H3TA,H3TB), C4T(H4TA,H4TB), C5T(H5TA,H5TB),
 C6T(H6TA,H6TB), C7T(H7TA,H7TB), C8T(H8TA,H8TB)
5.b 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), C2B(H2B), C3B(H3B),
  C4B(H4B), C5B(H5B), C6B(H6B), C8B(H8BA), C9B(H9B), C10B(H10B), C11B(H11B),
 C12B(H12B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C18B(H18B),
 C20B(H20B), C21B(H21C), C22B(H22C), C23B(H23B), C24B(H24B)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_hkl_checksum              79541
_shelx_res_checksum              7304
_shelxl_version_number           2013-3