Structural study of mono-, di- and tetranuclear complexes of the {Re(CO)3}+ fragment with thiosemicarbazone/thiosemicarbazonate ligands containing benzothiazole or benzoxazole groups
Pino-Cuevas, Arantxa; Graña, Ana; Abram, Ulrich; Carballo, Rosa; Vázquez-López, Ezequiel M.; CrystEngComm 20 (2018) 4781–; doi:10.1039/C8CE00874D

data_7231111
_publ_section_title
;
 Structural study of mono-, di- and tetranuclear complexes of the
 {Re(CO)3}+ fragment with thiosemicarbazone/thiosemicarbazonate ligands
 containing benzothiazole or benzoxazole groups
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4781
_journal_paper_doi               10.1039/C8CE00874D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C20 H16 Br N4 O5 Re S'
_chemical_formula_weight         690.54
_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
;
2018-03-09 deposited with the CCDC.
2018-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                65.0899(12)
_cell_angle_beta                 83.9903(15)
_cell_angle_gamma                89.3394(18)
_cell_formula_units_Z            2
_cell_length_a                   8.6134(3)
_cell_length_b                   11.6521(5)
_cell_length_c                   12.9674(5)
_cell_measurement_reflns_used    8147
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.97
_cell_measurement_theta_min      3.78
_cell_volume                     1173.13(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18464
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         68.747
_diffrn_reflns_theta_min         3.781
_exptl_absorpt_coefficient_mu    13.296
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0536P)^2^+3.7850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3959
_reflns_number_total             4074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00874d2.cif
_cod_data_source_block           8b_H2O
_cod_depositor_comments
'Adding full bibliography for 7231102--7231118.cif.'
_cod_original_cell_volume        1173.14(8)
_cod_database_code               7231111
_shelx_estimated_absorpt_t_min   0.197
_shelx_estimated_absorpt_t_max   0.498
_shelxl_version_number           2013-4
_shelx_res_checksum              36439