Phosphine-promoted ring-opening of benzisothiazolinate ligands at a nickel(ii) centre: a convenient synthesis of Ni(ii)-thiolate complexes.
Al-Jibori, Subhi A; Ali, Samer Hussein; Al-Janabi, Ahmed S; Wagner, Christoph; Hogarth, Graeme; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5520–5522; doi:10.1039/c9dt00953a

data_7049523
_publ_section_title
;
 Phosphine-promoted ring-opening of benzisothiazolinate ligands at a
 nickel(ii) centre: a convenient synthesis of Ni(ii)-thiolate complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5520
_journal_page_last               5522
_journal_paper_doi               10.1039/c9dt00953a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H31 N Ni O P2 S, 4(H2 O)'
_chemical_formula_sum            'C34 H39 N Ni O5 P2 S'
_chemical_formula_weight         694.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-04 deposited with the CCDC.    2019-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.392(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5162(7)
_cell_length_b                   13.4129(6)
_cell_length_c                   16.3229(6)
_cell_measurement_reflns_used    14264
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      1.99
_cell_volume                     3290.5(2)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19782
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.857
_diffrn_reflns_theta_min         1.991
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.7884
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(IPDS Software; Stoe & Cie, 1999)'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.452
_exptl_crystal_size_min          0.371
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1041P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4948
_reflns_number_total             6939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00953a2.cif
_cod_data_source_block           i2t1674
_cod_depositor_comments
'Adding full bibliography for 7049523--7049525.cif.'
_cod_database_code               7049523
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B), O3(H3A,H3B)
2.b Free rotating group:
 O4(H4A,H4B), O5(H5A,H5B)
2.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), N(H)
;
_shelx_res_checksum              75593
_olex2_submission_special_instructions 'No special instructions were received'