A bio-inspired mononuclear manganese catalyst for high-rate electrochemical hydrogen production.
Yang, Jie; He, Shuanglin; Wu, Qianqian; Zhang, Ping; Chen, Lin; Huang, Fang; Li, Fei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4783–4788; doi:10.1039/d1dt00672j

data_7706758
_publ_section_title
;
 A bio-inspired mononuclear manganese catalyst for high-rate
 electrochemical hydrogen production.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4783
_journal_page_last               4788
_journal_paper_doi               10.1039/d1dt00672j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C30 H19 Br Mn N3 O4, H2 O'
_chemical_formula_sum            'C30 H21 Br Mn N3 O5'
_chemical_formula_weight         638.35
_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     dual
_audit_creation_date             2020-07-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-10-14 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.758(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1335(3)
_cell_length_b                   27.4408(10)
_cell_length_c                   13.4270(6)
_cell_measurement_reflns_used    2152
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      72.8510
_cell_measurement_theta_min      3.1770
_cell_volume                     2627.08(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -58.00  -9.00   1.00    1.00    --  -40.98 125.00 150.00   49
  2  \w   -112.00 -43.00   1.00    1.00    --  -40.98 -57.00 -30.00   69
  3  \w    -93.00 -13.00   1.00    1.00    --  -40.98 -57.00  30.00   80
  4  \w     51.00  96.00   1.00    1.00    --   40.98-125.00 -90.00   45
  5  \w     68.00  97.00   1.00    2.00    --  106.95 -95.00 -90.00   29
  6  \w     27.00  54.00   1.00    2.00    --  106.95 -95.00 -90.00   27
  7  \w     34.00 121.00   1.00    2.00    --  106.95-125.00  90.00   87
  8  \w     66.00 131.00   1.00    2.00    --  106.95 -77.00 120.00   65
  9  \w     83.00 143.00   1.00    2.00    --  106.95  45.00   0.00   60
 10  \w     76.00 176.00   1.00    2.00    --  106.95  77.00 -60.00  100
 11  \w     87.00 146.00   1.00    2.00    --  106.95  45.00-150.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0607946000
_diffrn_orient_matrix_UB_12      0.0392557000
_diffrn_orient_matrix_UB_13      0.0763986000
_diffrn_orient_matrix_UB_21      -0.0215704000
_diffrn_orient_matrix_UB_22      -0.0370241000
_diffrn_orient_matrix_UB_23      0.0851272000
_diffrn_orient_matrix_UB_31      0.2062547000
_diffrn_orient_matrix_UB_32      -0.0154190000
_diffrn_orient_matrix_UB_33      -0.0098893000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9917
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.541
_diffrn_reflns_theta_min         3.221
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.513
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1234P)^2^+11.5231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3945
_reflns_number_total             5137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00672j2.cif
_cod_data_source_block           exp_2224
_cod_depositor_comments          'Adding full bibliography for 7706758.cif.'
_cod_database_code               7706758
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C24(H24), C25(H25),
  C26(H26), C27(H27)
;
_shelx_res_checksum              64266
_shelx_hkl_checksum              61022
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.665