Synthesis, structural studies, and redox chemistry of bimetallic [Mn(CO)<sub>3</sub>] and [Re(CO)<sub>3</sub>] complexes.
Henke, Wade C.; Kerr, Tyler A.; Sheridan, Thomas R.; Henling, Lawrence M.; Takase, Michael K.; Day, Victor W.; Gray, Harry B.; Blakemore, James D.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2746–2756; doi:10.1039/d0dt03666h

data_7706395
_publ_section_title
;
 Synthesis, structural studies, and redox chemistry of bimetallic
 [Mn(CO)<sub>3</sub>] and [Re(CO)<sub>3</sub>] complexes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2746
_journal_page_last               2756
_journal_paper_doi               10.1039/d0dt03666h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C14 H6 Br2 Mn2 N4 O6, 0.25(C12 O4)'
_chemical_formula_sum            'C17 H6 Br2 Mn2 N4 O7'
_chemical_formula_weight         647.96
_chemical_properties_physical    Light-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2021-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.597(3)
_cell_length_b                   10.830(2)
_cell_length_c                   11.8313(18)
_cell_measurement_reflns_used    1195
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      70.68
_cell_measurement_theta_min      4.79
_cell_volume                     2254.8(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4267
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         74.214
_diffrn_reflns_theta_min         4.794
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.687
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1178
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0632P)^2^+11.2199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                798
_reflns_number_total             1178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03666h3.cif
_cod_data_source_block           cmpd5syn_p15288
_cod_depositor_comments
'Adding full bibliography for 7706395--7706401.cif.'
_cod_database_code               7706395
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.341
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1S-C2S = C1S-C3S
 1.51 with sigma of 0.02
3. Restrained planarity
 O1S, C1S, C2S, C3S
 with sigma of 0.1
4. Rigid bond restraints
 O1S, C1S, C2S, C3S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
O1S \\sim C1S \\sim C2S \\sim C3S: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
6. Same fragment restrains
{O1S, C1S, C3S, C2S} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O1S, C1S, C2S, C3S}
7. Others
 Fixed Sof: C1S(0.25) C2S(0.25)
8.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
;
_shelx_res_checksum              39203
_olex2_submission_special_instructions 'No special instructions were received'