Mechanism of proton transfer to coordinated thiolates: encapsulation of acid stabilizes precursor intermediate.
Alwaaly, Ahmed; Clegg, William; Harrington, Ross W.; Petrou, Athinoula L.; Henderson, Richard A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11977–11983; doi:10.1039/c5dt01716e

data_7035361
_publ_section_title
;
 Mechanism of proton transfer to coordinated thiolates: encapsulation of
 acid stabilizes precursor intermediate.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11977
_journal_page_last               11983
_journal_paper_doi               10.1039/c5dt01716e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C38 H42 Ni P3 S +,C24 H20 B -,0.5 C H2 Cl2'
_chemical_formula_sum            'C62.5 H63 B Cl Ni P3 S'
_chemical_formula_weight         1044.07
_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
_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2015-01-10 deposited with the CCDC.
2015-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                72.371(4)
_cell_angle_beta                 75.534(4)
_cell_angle_gamma                67.285(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5663(6)
_cell_length_b                   13.8894(6)
_cell_length_c                   17.6784(8)
_cell_measurement_reflns_used    6673
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.98
_cell_volume                     2681.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.987
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1098
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and methanol'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         10556
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0538P)^2^+2.1060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7732
_reflns_number_total             10556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01716e2.cif
_cod_data_source_block           rah213
_cod_depositor_comments
'Adding full bibliography for 7035360--7035362.cif.'
_cod_database_code               7035361
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              57850