The crystal structure of (azido)-κ1 N-6,6′-((cyclohexane-1,2-diylbis(azanylylidene)) bis(methanylylidene))bis(3-bromophenolato- κ 4 N,N,O,O)-(methanol)-manganese(III)–methanol(1/1), C 22 H 26 Br 2 MnN 5 O 4
Liu, Dian; Ma, Xun; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 623–625; doi:10.1515/ncrs-2021-0014

data_8104784
_publ_section_title
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 The crystal structure of (azido)-\k1
 N-6,6&#x2032;-((cyclohexane-1,2-diylbis(azanylylidene))
 bis(methanylylidene))bis(3-bromophenolato- \k 4
 N,N,O,O)-(methanol)-manganese(III)--methanol(1/1), C 22 H 26 Br 2 MnN 5 O
 4
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_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              623
_journal_page_last               625
_journal_paper_doi               10.1515/ncrs-2021-0014
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C21 H22 Br2 Mn N5 O3, C H4 O'
_chemical_formula_sum            'C22 H26 Br2 Mn N5 O4'
_chemical_formula_weight         639.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 100.330(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0106(4)
_cell_length_b                   14.5925(7)
_cell_length_c                   21.0425(11)
_cell_measurement_reflns_used    7217
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.396
_cell_measurement_theta_min      2.413
_cell_volume                     2419.9(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21493
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         2.412
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.887
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.5948.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5556
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0285P)^2^+1.1719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4352
_reflns_number_total             5556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0014_suppl.cif
_cod_data_source_block           1
_cod_database_code               8104784
_shelx_estimated_absorpt_t_max   0.575
_shelx_estimated_absorpt_t_min   0.510
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C21-H3
 1.897861 with sigma of 0.02
 Mn3-H3
 2.977788 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C7(H7), C14(H14), C16(H16), C17(H17), C18(H18)
3.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
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_olex2_submission_special_instructions 'No special instructions were received'