Co-ordination behaviour of a novel tristhiourea tripodal ligand; structural variations in a series of transition metal complexes.
Saad, Fawaz A.; Knight, James C.; Kariuki, Benson M.; Amoroso, Angelo J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10280–10288; doi:10.1039/c6dt01148a

data_7040207
_publ_section_title
;
 Co-ordination behaviour of a novel tristhiourea tripodal ligand;
 structural variations in a series of transition metal complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10280
_journal_page_last               10288
_journal_paper_doi               10.1039/c6dt01148a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C51.2 H50.6 Cl2 N14.6 Ni O11.4 S3'
_chemical_formula_weight         1278.65
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-22 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                107.831(2)
_cell_angle_beta                 97.828(2)
_cell_angle_gamma                94.342(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8450(5)
_cell_length_b                   14.6430(5)
_cell_length_c                   15.8030(6)
_cell_measurement_reflns_used    6566
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.92
_cell_volume                     2997.95(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_unetI/netI     0.1650
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_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            25225
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.9436
_exptl_absorpt_correction_T_min  0.8671
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Denzo/Scalepack
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       needle
_exptl_crystal_F_000             1322
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13501
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1942
_refine_ls_R_factor_gt           0.0931
_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^)+(0.1189P)^2^+0.6118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6559
_reflns_number_total             13501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01148a2.cif
_cod_data_source_block           aja0821
_cod_original_formula_sum        'C51.20 H50.60 Cl2 N14.60 Ni O11.40 S3'
_cod_database_code               7040207
_shelx_estimated_absorpt_t_min   0.867
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2013-4
_shelx_res_checksum              4750