The crystal structure of [μ-hydroxido-bis[(5,5′-dimethyl-2,2′-bipyridine-κ2 N,N′)-tricarbonylrhenium(I)] bromide hemihydrate, C30H26N4O9Re2Br
Moherane, Lehlohonolo; Alexander, Orbett T.; Visser, Hendrik G.; Manicum, Amanda-Lee E.; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1027–1029; doi:10.1515/ncrs-2021-0210

data_8104657
_publ_section_title
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 The crystal structure of
 [\m-hydroxido-bis[(5,5&#x2032;-dimethyl-2,2&#x2032;-bipyridine-\k2
 N,N&#x2032;)-tricarbonylrhenium(I)] bromide hemihydrate, C30H26N4O9Re2Br
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1027
_journal_page_last               1029
_journal_paper_doi               10.1515/ncrs-2021-0210
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         '0.5(C30 H25 N4 O7 Re2), 0.5(Br), 0.25(H2 O)'
_chemical_formula_sum            'C15 H13 Br0.5 N2 O3.75 Re'
_chemical_formula_weight         507.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                82.700(2)
_cell_angle_beta                 76.682(2)
_cell_angle_gamma                77.364(2)
_cell_formula_units_Z            4
_cell_length_a                   9.4069(6)
_cell_length_b                   11.7695(8)
_cell_length_c                   15.0549(11)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      3.15
_cell_volume                     1577.52(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66539
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         1.779
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.987
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1510 before and 0.1057 after correction.
The Ratio of minimum to maximum transmission is 0.5678.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       Plate
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.767
_refine_diff_density_min         -1.713
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+1.3040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7101
_reflns_number_total             7825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0210_suppl.cif
_cod_data_source_block           mo_v4_21olam1_0m
_cod_original_formula_sum        'C15 H13 Br0.50 N2 O3.75 Re'
_cod_database_code               8104657
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.134
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5)
3.a Free rotating group:
 O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13), C16(H16),
 C17(H17), C20(H20), C21(H21), C24(H24)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C)
;