Crystal structure of fac-tricarbonyl-(nitrato-k1 O)-bis(pyridine-κN)-rhenium, C13H10O6N3Re
Jacobs, Francois J. F.; Brink, Alice; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 253–255; doi:10.1515/ncrs-2020-0475

data_8104937
_publ_section_title
;
 Crystal structure of fac-tricarbonyl-(nitrato-k1
 O)-bis(pyridine-\kN)-rhenium, C13H10O6N3Re
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              253
_journal_page_last               255
_journal_paper_doi               10.1515/ncrs-2020-0475
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C13 H10 N3 O6 Re'
_chemical_formula_sum            'C13 H10 N3 O6 Re'
_chemical_formula_weight         490.44
_chemical_name_systematic
fac-Tricarbonyl-(nitrato)-bis(pyridine-N)-rhenium
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_cell_angle_alpha                90
_cell_angle_beta                 92.637(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9325(9)
_cell_length_b                   13.8112(16)
_cell_length_c                   13.4577(15)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    101.0
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.57
_cell_volume                     1472.8(3)
_computing_cell_refinement       'Apex3 (Bruker AXS Inc., 2016)'
_computing_data_collection       'Apex3 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'Apex3 (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Mercury 4.0 (MacRae et al., 2020)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 Quest Eco Chi Photon II CPAD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.286
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int)
 was 0.1079 before and 0.0779 after correction. The Ratio of minimum to 
 maximum transmission is 0.8069. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_description       Cuboid
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.892
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+3.2025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3221
_reflns_number_total             3551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0475_suppl.cif
_cod_data_source_block           q1_20ffj4_0m
_cod_database_code               8104937
_shelx_estimated_absorpt_t_max   0.529
_shelx_estimated_absorpt_t_min   0.436
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13)
;