#------------------------------------------------------------------------------
#$Date: 2020-02-25 01:44:24 +0200 (Tue, 25 Feb 2020) $
#$Revision: 248421 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/42/4134233.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4134233
loop_
_publ_author_name
'Rønne, Magnus Haugaard H'
'Cho, Dasol'
'Madsen, Monica R.'
'Jakobsen, Joakim B.'
'Eom, Seunghwan'
'Escoudé, Émile'
'Hammershøj, Hans Christian D'
'Nielsen, Dennis U.'
'Pedersen, Steen U.'
'Baik, Mu-Hyun'
'Skrydstrup, Troels'
'Daasbjerg, Kim'
_publ_section_title
;
 Ligand Controlled Product Selectivity in the Electrochemical Carbon
 Dioxide Reduction Using Manganese Bipyridine Catalysts.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11806
_journal_year                    2020
_chemical_formula_moiety         'C35 H38 Br Mn N4 O3'
_chemical_formula_sum            'C35 H38 Br Mn N4 O3'
_chemical_formula_weight         697.54
_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     direct
_audit_creation_date             2019-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.9199(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4608(2)
_cell_length_b                   29.8404(5)
_cell_length_c                   17.2593(3)
_cell_measurement_reflns_used    24263
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.9520
_cell_measurement_theta_min      1.7950
_cell_volume                     6729.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3590
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      7.00  87.00   1.00   30.00    --   18.69-132.00 -23.00   80
  2  ω     10.00  90.00   1.00   30.00    --   18.69-137.00 159.00   80
  3  ω    -91.00 -10.00   1.00   30.00    --  -19.47 137.00-137.00   81
  4  ω    -88.00  -7.00   1.00   30.00    --  -19.47 132.00  45.00   81
  5  ω    -82.00 -35.00   1.00   30.00    --   18.69-178.00-180.00   47
  6  ω    -28.00 109.00   1.00   30.00    --   18.69  38.00 -90.00  137
  7  ω    -73.00 -48.00   1.00   30.00    --   18.69 -57.00 150.00   25
  8  ω    -28.00 109.00   1.00   30.00    --   18.69  38.00 120.00  137
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004982000
_diffrn_orient_matrix_UB_12      -0.0231374000
_diffrn_orient_matrix_UB_13      -0.0095132000
_diffrn_orient_matrix_UB_21      -0.0017668000
_diffrn_orient_matrix_UB_22      -0.0053862000
_diffrn_orient_matrix_UB_23      0.0396847000
_diffrn_orient_matrix_UB_31      -0.0542395000
_diffrn_orient_matrix_UB_32      0.0004000000
_diffrn_orient_matrix_UB_33      -0.0113923000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            84269
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.701
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.994
_refine_diff_density_min         -1.996
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         13754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0874P)²+20.5498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11132
_reflns_number_total             13754
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b11806_si_002.cif
_cod_data_source_block           magnus_1
_cod_database_code               4134233
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'Mn C35 H38 N4 O3'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C7B) = Uanis(C7A)
3.a Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C6A(H6AA,H6AB), C8A(H8AA,H8AB), C32A(H32A,H32B), C34A(H34A,
 H34B), C35A(H35A,H35B), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C8B(H8BA,H8BB),
 C31B(H31A,H31B), C33B(H33D,H33E), C34B(H34C,H34D)
3.b Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C16A(H16A), C17A(H17A),
 C18A(H18A), C21A(H21A), C22A(H22A), C23A(H23A), C26A(H26A), C27A(H27A),
 C28A(H28A), C29A(H29A), C10B(H10B), C11B(H11B), C12B(H12B), C13B(H13B),
 C16B(H16B), C17B(H17B), C18B(H18B), C21B(H21B), C22B(H22B), C23B(H23B),
 C26B(H26B), C27B(H27B), C28B(H28B), C29B(H29B)
3.c Idealised Me refined with riding coordinates:
 C7B(H7BA,H7BB,H7BC)
3.d Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C7A(H7AA,H7AB,H7AC), C33A(H33A,H33B,H33C), C36A(H36A,
 H36B,H36C), C4B(H4BA,H4BB,H4BC), C32B(H32C,H32D,H32E), C35B(H35C,H35D,H35E)
;
_olex2_date_sample_data_collection 2019-02-22
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.896
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1A Br 0.64735(4) 0.75318(2) 0.28735(3) 0.03429(13) Uani 1 1 d . . . . .
Mn1A Mn 0.76615(5) 0.69392(2) 0.25640(4) 0.02516(15) Uani 1 1 d . . . . .
O1A O 0.6064(2) 0.62781(12) 0.2635(2) 0.0376(8) Uani 1 1 d . . . . .
O2A O 0.8117(2) 0.66179(10) 0.42265(17) 0.0316(7) Uani 1 1 d . . . . .
O3A O 0.9042(2) 0.62534(11) 0.2203(2) 0.0353(7) Uani 1 1 d . . . . .
N1A N 0.3529(4) 0.7039(2) 0.1128(4) 0.0751(17) Uani 1 1 d . . . . .
N2A N 0.7221(3) 0.71711(12) 0.1401(2) 0.0283(8) Uani 1 1 d . . . . .
N3A N 0.8709(3) 0.74567(12) 0.2605(2) 0.0268(8) Uani 1 1 d . . . . .
N4A N 0.9615(3) 0.82071(14) 0.4752(3) 0.0376(9) Uani 1 1 d . . . . .
C1A C 0.8513(4) 0.65141(15) 0.2330(3) 0.0304(10) Uani 1 1 d . . . . .
C2A C 0.6651(3) 0.65372(16) 0.2542(2) 0.0290(9) Uani 1 1 d . . . . .
C3A C 0.7999(3) 0.67686(14) 0.3600(3) 0.0275(9) Uani 1 1 d . . . . .
C4A C 0.8045(4) 0.8606(2) 0.4031(4) 0.0563(15) Uani 1 1 d . . . . .
H4AA H 0.834339 0.866410 0.358872 0.084 Uiso 1 1 calc GR . . . .
H4AB H 0.760246 0.885038 0.408743 0.084 Uiso 1 1 calc GR . . . .
H4AC H 0.765557 0.833381 0.393696 0.084 Uiso 1 1 calc GR . . . .
C5A C 0.8879(4) 0.8561(2) 0.4782(4) 0.0511(14) Uani 1 1 d . . . . .
H5AA H 0.924108 0.884392 0.488800 0.061 Uiso 1 1 calc R . . . .
H5AB H 0.856831 0.850178 0.522426 0.061 Uiso 1 1 calc R . . . .
C6A C 1.0553(4) 0.82638(19) 0.5381(3) 0.0446(12) Uani 1 1 d . . . . .
H6AA H 1.093012 0.798392 0.545637 0.054 Uiso 1 1 calc R . . . .
H6AB H 1.037526 0.833746 0.587804 0.054 Uiso 1 1 calc R . . . .
C7A C 1.1230(7) 0.8634(3) 0.5175(6) 0.0902(18) Uani 1 1 d . . . . .
H7AA H 1.129500 0.859351 0.463701 0.135 Uiso 1 1 calc GR . . . .
H7AB H 1.189534 0.861926 0.553482 0.135 Uiso 1 1 calc GR . . . .
H7AC H 1.092707 0.892018 0.522253 0.135 Uiso 1 1 calc GR . . . .
C8A C 0.9160(4) 0.77655(19) 0.4810(3) 0.0452(13) Uani 1 1 d . . . . .
H8AA H 0.849649 0.775533 0.443436 0.054 Uiso 1 1 calc R . . . .
H8AB H 0.904691 0.773395 0.534143 0.054 Uiso 1 1 calc R . . . .
C9A C 0.9778(4) 0.73713(17) 0.4652(3) 0.0392(11) Uani 1 1 d . . . . .
C10A C 1.0202(5) 0.7069(2) 0.5265(3) 0.0572(17) Uani 1 1 d . . . . .
H10A H 1.013498 0.712853 0.577887 0.069 Uiso 1 1 calc R . . . .
C11A C 1.0711(6) 0.6690(2) 0.5133(4) 0.070(2) Uani 1 1 d . . . . .
H11A H 1.097083 0.649419 0.555311 0.085 Uiso 1 1 calc R . . . .
C12A C 1.0841(5) 0.6595(2) 0.4369(4) 0.0659(19) Uani 1 1 d . . . . .
H12A H 1.120002 0.634160 0.427929 0.079 Uiso 1 1 calc R . . . .
C13A C 1.0430(4) 0.68828(17) 0.3754(4) 0.0472(13) Uani 1 1 d . . . . .
H13A H 1.050774 0.682336 0.324284 0.057 Uiso 1 1 calc R . . . .
C14A C 0.9895(4) 0.72650(16) 0.3892(3) 0.0357(10) Uani 1 1 d . . . . .
C15A C 0.9509(4) 0.75723(15) 0.3206(3) 0.0305(9) Uani 1 1 d . . . . .
C16A C 1.0036(4) 0.79753(16) 0.3196(3) 0.0369(11) Uani 1 1 d . . . . .
H16A H 1.059258 0.804534 0.361301 0.044 Uiso 1 1 calc R . . . .
C17A C 0.9730(4) 0.82670(17) 0.2570(3) 0.0416(12) Uani 1 1 d . . . . .
H17A H 1.006041 0.854049 0.256749 0.050 Uiso 1 1 calc R . . . .
C18A C 0.8925(4) 0.81490(16) 0.1943(3) 0.0384(11) Uani 1 1 d . . . . .
H18A H 0.870592 0.834006 0.150994 0.046 Uiso 1 1 calc R . . . .
C19A C 0.8445(4) 0.77366(15) 0.1973(3) 0.0300(9) Uani 1 1 d . . . . .
C20A C 0.7651(4) 0.75734(15) 0.1300(3) 0.0304(9) Uani 1 1 d . . . . .
C21A C 0.7379(4) 0.78084(16) 0.0578(3) 0.0360(11) Uani 1 1 d . . . . .
H21A H 0.766495 0.808743 0.052754 0.043 Uiso 1 1 calc R . . . .
C22A C 0.6681(4) 0.76209(17) -0.0059(3) 0.0374(11) Uani 1 1 d . . . . .
H22A H 0.649115 0.777112 -0.054438 0.045 Uiso 1 1 calc R . . . .
C23A C 0.6275(4) 0.72125(17) 0.0035(3) 0.0366(11) Uani 1 1 d . . . . .
H23A H 0.582136 0.707837 -0.039426 0.044 Uiso 1 1 calc R . . . .
C24A C 0.6532(4) 0.69929(15) 0.0772(3) 0.0309(9) Uani 1 1 d . . . . .
C25A C 0.6009(3) 0.65629(17) 0.0844(3) 0.0315(10) Uani 1 1 d . . . . .
C26A C 0.6489(3) 0.61560(16) 0.0791(3) 0.0314(10) Uani 1 1 d . . . . .
H26A H 0.716817 0.615174 0.075775 0.038 Uiso 1 1 calc R . . . .
C27A C 0.5963(4) 0.57548(17) 0.0789(3) 0.0367(11) Uani 1 1 d . . . . .
H27A H 0.628965 0.548253 0.076298 0.044 Uiso 1 1 calc R . . . .
C28A C 0.4950(4) 0.5766(2) 0.0824(3) 0.0457(13) Uani 1 1 d . . . . .
H28A H 0.458869 0.549955 0.081855 0.055 Uiso 1 1 calc R . . . .
C29A C 0.4468(4) 0.6172(2) 0.0869(3) 0.0447(13) Uani 1 1 d . . . . .
H29A H 0.378401 0.617507 0.088877 0.054 Uiso 1 1 calc R . . . .
C30A C 0.4984(4) 0.65746(19) 0.0883(3) 0.0398(12) Uani 1 1 d . . . . .
C32A C 0.4469(5) 0.7024(2) 0.0946(4) 0.0612(18) Uani 1 1 d . . . . .
H32A H 0.493837 0.719993 0.134670 0.073 Uiso 1 1 calc R . . . .
H32B H 0.440116 0.717760 0.044075 0.073 Uiso 1 1 calc R . . . .
C33A C 0.2663(8) 0.7451(4) -0.0072(7) 0.136(5) Uani 1 1 d . . . . .
H33A H 0.311042 0.763758 -0.028908 0.204 Uiso 1 1 calc GR . . . .
H33B H 0.197418 0.756079 -0.024238 0.204 Uiso 1 1 calc GR . . . .
H33C H 0.269338 0.714918 -0.025638 0.204 Uiso 1 1 calc GR . . . .
C34A C 0.2993(7) 0.7461(3) 0.0827(6) 0.100(3) Uani 1 1 d . . . . .
H34A H 0.344646 0.771330 0.099755 0.120 Uiso 1 1 calc R . . . .
H34B H 0.239872 0.749719 0.104552 0.120 Uiso 1 1 calc R . . . .
C35A C 0.3692(6) 0.7002(3) 0.2027(5) 0.079(2) Uani 1 1 d . . . . .
H35A H 0.391432 0.729049 0.226568 0.095 Uiso 1 1 calc R . . . .
H35B H 0.423504 0.678774 0.222723 0.095 Uiso 1 1 calc R . . . .
C36A C 0.2718(7) 0.6854(4) 0.2290(6) 0.096(3) Uani 1 1 d . . . . .
H36A H 0.223425 0.709576 0.220833 0.145 Uiso 1 1 calc GR . . . .
H36B H 0.289893 0.677383 0.284494 0.145 Uiso 1 1 calc GR . . . .
H36C H 0.241794 0.659951 0.197906 0.145 Uiso 1 1 calc GR . . . .
Br1B Br 0.06504(3) 0.43016(2) 0.35648(3) 0.02879(12) Uani 1 1 d . . . . .
Mn1B Mn 0.07946(4) 0.49651(2) 0.26792(4) 0.02356(15) Uani 1 1 d . . . . .
O1B O 0.0997(3) 0.57282(14) 0.1642(2) 0.0507(10) Uani 1 1 d . . . . .
O2B O 0.2612(2) 0.45970(14) 0.2235(2) 0.0494(10) Uani 1 1 d . . . . .
O3B O -0.0011(3) 0.43757(13) 0.1295(2) 0.0446(9) Uani 1 1 d . . . . .
N1B N -0.3289(4) 0.40496(17) 0.1837(3) 0.0555(13) Uani 1 1 d . . . . .
N2B N -0.0520(2) 0.52130(11) 0.2944(2) 0.0234(7) Uani 1 1 d . . . . .
N3B N 0.1406(2) 0.52894(11) 0.3750(2) 0.0232(7) Uani 1 1 d . . . . .
N4B N 0.4631(3) 0.42344(16) 0.4362(3) 0.0534(12) Uani 1 1 d . . . . .
C1B C 0.0901(3) 0.54327(18) 0.2049(3) 0.0361(11) Uani 1 1 d . . . . .
C2B C 0.1955(3) 0.47480(17) 0.2467(3) 0.0334(10) Uani 1 1 d . . . . .
C3B C 0.0225(3) 0.46180(16) 0.1824(3) 0.0308(10) Uani 1 1 d . . . . .
C4B C -0.5159(7) 0.4032(6) 0.1384(5) 0.192(9) Uani 1 1 d . . . . .
H4BA H -0.525660 0.379152 0.172695 0.288 Uiso 1 1 calc GR . . . .
H4BB H -0.506657 0.391227 0.089040 0.288 Uiso 1 1 calc GR . . . .
H4BC H -0.574902 0.422427 0.127921 0.288 Uiso 1 1 calc GR . . . .
C5B C -0.4198(4) 0.4306(3) 0.1798(4) 0.074(2) Uani 1 1 d . . . . .
H5BA H -0.417093 0.458021 0.150137 0.089 Uiso 1 1 calc R . . . .
H5BB H -0.424168 0.438700 0.233284 0.089 Uiso 1 1 calc R . . . .
C6B C -0.3238(7) 0.3673(3) 0.2415(8) 0.111(4) Uani 1 1 d . . . . .
H6BA H -0.379407 0.346770 0.219945 0.133 Uiso 1 1 calc R . . . .
H6BB H -0.335623 0.379483 0.290622 0.133 Uiso 1 1 calc R . . . .
C7B C -0.2218(7) 0.3399(3) 0.2627(6) 0.0902(18) Uani 1 1 d . . . . .
H7BA H -0.226905 0.316718 0.300186 0.135 Uiso 1 1 calc R . . . .
H7BB H -0.165983 0.359440 0.285783 0.135 Uiso 1 1 calc R . . . .
H7BC H -0.210028 0.326541 0.215044 0.135 Uiso 1 1 calc R . . . .
C8B C -0.2399(4) 0.4330(2) 0.2075(4) 0.0572(17) Uani 1 1 d . . . . .
H8BA H -0.180077 0.413973 0.223892 0.069 Uiso 1 1 calc R . . . .
H8BB H -0.245904 0.450453 0.253530 0.069 Uiso 1 1 calc R . . . .
C9B C -0.2229(3) 0.46492(17) 0.1430(3) 0.0365(11) Uani 1 1 d . . . . .
C10B C -0.2497(4) 0.45228(18) 0.0630(3) 0.0435(13) Uani 1 1 d . . . . .
H10B H -0.284394 0.425456 0.048612 0.052 Uiso 1 1 calc R . . . .
C11B C -0.2257(4) 0.47882(19) 0.0051(3) 0.0435(12) Uani 1 1 d . . . . .
H11B H -0.244406 0.469802 -0.048019 0.052 Uiso 1 1 calc R . . . .
C12B C -0.1744(4) 0.51852(18) 0.0249(3) 0.0385(11) Uani 1 1 d . . . . .
H12B H -0.157499 0.536099 -0.014595 0.046 Uiso 1 1 calc R . . . .
C13B C -0.1477(3) 0.53235(15) 0.1041(3) 0.0304(9) Uani 1 1 d . . . . .
H13B H -0.113877 0.559468 0.117416 0.036 Uiso 1 1 calc R . . . .
C14B C -0.1713(3) 0.50592(15) 0.1634(3) 0.0292(9) Uani 1 1 d . . . . .
C15B C -0.1489(3) 0.52230(14) 0.2470(3) 0.0262(9) Uani 1 1 d . . . . .
C16B C -0.2303(3) 0.53959(16) 0.2760(3) 0.0331(10) Uani 1 1 d . . . . .
H16B H -0.296051 0.540040 0.243077 0.040 Uiso 1 1 calc R . . . .
C17B C -0.2137(3) 0.55565(16) 0.3518(3) 0.0345(10) Uani 1 1 d . . . . .
H17B H -0.267641 0.566989 0.370814 0.041 Uiso 1 1 calc R . . . .
C18B C -0.1159(3) 0.55492(15) 0.4001(3) 0.0296(9) Uani 1 1 d . . . . .
H18B H -0.102847 0.565827 0.452086 0.036 Uiso 1 1 calc R . . . .
C19B C -0.0374(3) 0.53768(14) 0.3700(2) 0.0232(8) Uani 1 1 d . . . . .
C20B C 0.0698(3) 0.53775(13) 0.4168(2) 0.0233(8) Uani 1 1 d . . . . .
C21B C 0.0957(3) 0.54735(14) 0.4979(3) 0.0282(9) Uani 1 1 d . . . . .
H21B H 0.045003 0.552121 0.525302 0.034 Uiso 1 1 calc R . . . .
C22B C 0.1979(3) 0.54972(15) 0.5373(3) 0.0319(10) Uani 1 1 d . . . . .
H22B H 0.217206 0.555105 0.591971 0.038 Uiso 1 1 calc R . . . .
C23B C 0.2704(3) 0.54399(16) 0.4943(3) 0.0319(10) Uani 1 1 d . . . . .
H23B H 0.339426 0.547084 0.519168 0.038 Uiso 1 1 calc R . . . .
C24B C 0.2408(3) 0.53356(14) 0.4137(3) 0.0274(9) Uani 1 1 d . . . . .
C25B C 0.3206(3) 0.53123(17) 0.3668(3) 0.0339(10) Uani 1 1 d . . . . .
C26B C 0.3234(4) 0.56552(19) 0.3122(3) 0.0398(11) Uani 1 1 d . . . . .
H26B H 0.272243 0.587198 0.302668 0.048 Uiso 1 1 calc R . . . .
C27B C 0.3999(4) 0.5679(2) 0.2722(3) 0.0488(14) Uani 1 1 d . . . . .
H27B H 0.400300 0.590654 0.235522 0.059 Uiso 1 1 calc R . . . .
C28B C 0.4758(4) 0.5362(2) 0.2872(4) 0.0537(15) Uani 1 1 d . . . . .
H28B H 0.528175 0.537639 0.260602 0.064 Uiso 1 1 calc R . . . .
C29B C 0.4753(4) 0.5023(2) 0.3411(3) 0.0459(13) Uani 1 1 d . . . . .
H29B H 0.527904 0.481285 0.350391 0.055 Uiso 1 1 calc R . . . .
C30B C 0.3973(3) 0.49850(18) 0.3827(3) 0.0367(11) Uani 1 1 d . . . . .
C31B C 0.3938(4) 0.46055(18) 0.4409(3) 0.0425(12) Uani 1 1 d . . . . .
H31A H 0.411059 0.472444 0.494821 0.051 Uiso 1 1 calc R . . . .
H31B H 0.324381 0.449103 0.430596 0.051 Uiso 1 1 calc R . . . .
C32B C 0.5481(8) 0.3568(3) 0.5163(10) 0.161(7) Uani 1 1 d . . . . .
H32C H 0.525409 0.336295 0.472756 0.242 Uiso 1 1 calc GR . . . .
H32D H 0.551098 0.341610 0.565823 0.242 Uiso 1 1 calc GR . . . .
H32E H 0.614905 0.367854 0.515679 0.242 Uiso 1 1 calc GR . . . .
C33B C 0.4736(5) 0.3958(2) 0.5077(5) 0.071(2) Uani 1 1 d . . . . .
H33D H 0.406626 0.384015 0.508336 0.085 Uiso 1 1 calc R . . . .
H33E H 0.495024 0.415032 0.554075 0.085 Uiso 1 1 calc R . . . .
C34B C 0.4322(7) 0.3975(3) 0.3609(5) 0.086(3) Uani 1 1 d . . . . .
H34C H 0.424976 0.418806 0.317463 0.103 Uiso 1 1 calc R . . . .
H34D H 0.489418 0.378250 0.358426 0.103 Uiso 1 1 calc R . . . .
C35B C 0.3452(7) 0.3709(3) 0.3440(7) 0.103(3) Uani 1 1 d . . . . .
H35C H 0.352849 0.347101 0.382468 0.155 Uiso 1 1 calc GR . . . .
H35D H 0.335975 0.358339 0.291498 0.155 Uiso 1 1 calc GR . . . .
H35E H 0.286665 0.388708 0.346276 0.155 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 5 0 0.0653
0 -4 5 0.0565
-5 -1 2 0.0741
5 1 -2 0.0741
2 -4 5 0.0702
1 -5 -4 0.0574
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2A Mn1A Br1A 85.58(10) . . ?
N2A Mn1A N3A 79.57(15) . . ?
N3A Mn1A Br1A 86.06(10) . . ?
C1A Mn1A Br1A 179.39(14) . . ?
C1A Mn1A N2A 93.82(16) . . ?
C1A Mn1A N3A 93.87(17) . . ?
C2A Mn1A Br1A 87.58(14) . . ?
C2A Mn1A N2A 99.35(17) . . ?
C2A Mn1A N3A 173.61(17) . . ?
C2A Mn1A C1A 92.5(2) . . ?
C2A Mn1A C3A 80.97(19) . . ?
C3A Mn1A Br1A 90.53(14) . . ?
C3A Mn1A N2A 176.07(17) . . ?
C3A Mn1A N3A 99.68(17) . . ?
C3A Mn1A C1A 90.08(19) . . ?
C32A N1A C34A 110.1(7) . . ?
C32A N1A C35A 108.4(5) . . ?
C34A N1A C35A 111.1(7) . . ?
C20A N2A Mn1A 112.8(3) . . ?
C24A N2A Mn1A 128.8(3) . . ?
C24A N2A C20A 118.3(4) . . ?
C15A N3A Mn1A 128.8(3) . . ?
C15A N3A C19A 117.9(4) . . ?
C19A N3A Mn1A 112.8(3) . . ?
C5A N4A C6A 111.2(4) . . ?
C5A N4A C8A 110.5(4) . . ?
C6A N4A C8A 110.7(4) . . ?
O3A C1A Mn1A 178.6(4) . . ?
O1A C2A Mn1A 170.8(4) . . ?
O2A C3A Mn1A 171.0(4) . . ?
N4A C5A C4A 114.0(5) . . ?
N4A C6A C7A 111.6(5) . . ?
N4A C8A C9A 115.6(4) . . ?
C10A C9A C8A 120.6(5) . . ?
C14A C9A C8A 122.8(4) . . ?
C14A C9A C10A 116.5(5) . . ?
C11A C10A C9A 122.4(6) . . ?
C10A C11A C12A 120.2(5) . . ?
C13A C12A C11A 118.9(6) . . ?
C12A C13A C14A 120.4(6) . . ?
C9A C14A C13A 121.7(5) . . ?
C9A C14A C15A 120.8(4) . . ?
C13A C14A C15A 117.4(5) . . ?
N3A C15A C14A 121.0(4) . . ?
N3A C15A C16A 121.6(4) . . ?
C16A C15A C14A 117.3(4) . . ?
C17A C16A C15A 119.9(5) . . ?
C16A C17A C18A 119.1(5) . . ?
C17A C18A C19A 118.6(4) . . ?
N3A C19A C18A 122.7(4) . . ?
N3A C19A C20A 115.8(4) . . ?
C18A C19A C20A 121.4(4) . . ?
N2A C20A C19A 116.4(4) . . ?
N2A C20A C21A 121.8(4) . . ?
C21A C20A C19A 121.8(4) . . ?
C22A C21A C20A 119.2(5) . . ?
C23A C22A C21A 118.9(4) . . ?
C22A C23A C24A 120.6(5) . . ?
N2A C24A C23A 121.1(4) . . ?
N2A C24A C25A 121.3(4) . . ?
C23A C24A C25A 117.6(4) . . ?
C26A C25A C24A 120.9(4) . . ?
C26A C25A C30A 120.3(5) . . ?
C30A C25A C24A 118.5(4) . . ?
C25A C26A C27A 120.6(4) . . ?
C28A C27A C26A 119.2(5) . . ?
C27A C28A C29A 120.2(5) . . ?
C30A C29A C28A 121.4(5) . . ?
C25A C30A C32A 119.7(5) . . ?
C29A C30A C25A 118.3(5) . . ?
C29A C30A C32A 122.0(5) . . ?
N1A C32A C30A 120.2(7) . . ?
N1A C34A C33A 110.1(8) . . ?
N1A C35A C36A 113.3(6) . . ?
N2B Mn1B Br1B 87.28(10) . . ?
N2B Mn1B N3B 79.26(13) . . ?
N3B Mn1B Br1B 84.20(10) . . ?
C1B Mn1B Br1B 179.64(17) . . ?
C1B Mn1B N2B 93.05(18) . . ?
C1B Mn1B N3B 96.00(18) . . ?
C1B Mn1B C2B 87.5(2) . . ?
C1B Mn1B C3B 91.8(2) . . ?
C2B Mn1B Br1B 92.14(16) . . ?
C2B Mn1B N2B 178.94(17) . . ?
C2B Mn1B N3B 99.80(16) . . ?
C2B Mn1B C3B 81.24(19) . . ?
C3B Mn1B Br1B 88.04(15) . . ?
C3B Mn1B N2B 99.62(16) . . ?
C3B Mn1B N3B 172.20(18) . . ?
C5B N1B C6B 109.5(5) . . ?
C5B N1B C8B 110.3(5) . . ?
C8B N1B C6B 110.2(6) . . ?
C15B N2B Mn1B 128.4(3) . . ?
C15B N2B C19B 117.6(4) . . ?
C19B N2B Mn1B 113.9(3) . . ?
C20B N3B Mn1B 112.7(3) . . ?
C20B N3B C24B 117.4(4) . . ?
C24B N3B Mn1B 128.3(3) . . ?
C31B N4B C34B 113.4(5) . . ?
C33B N4B C31B 108.2(5) . . ?
C33B N4B C34B 113.3(6) . . ?
O1B C1B Mn1B 178.0(5) . . ?
O2B C2B Mn1B 170.9(4) . . ?
O3B C3B Mn1B 171.1(4) . . ?
N1B C5B C4B 110.4(9) . . ?
N1B C6B C7B 116.5(6) . . ?
N1B C8B C9B 114.6(5) . . ?
C10B C9B C8B 120.4(5) . . ?
C10B C9B C14B 118.5(5) . . ?
C14B C9B C8B 120.8(5) . . ?
C11B C10B C9B 121.0(5) . . ?
C12B C11B C10B 120.6(5) . . ?
C11B C12B C13B 119.7(5) . . ?
C14B C13B C12B 120.4(4) . . ?
C9B C14B C15B 120.1(4) . . ?
C13B C14B C9B 119.7(4) . . ?
C13B C14B C15B 120.1(4) . . ?
N2B C15B C14B 121.1(4) . . ?
N2B C15B C16B 120.6(4) . . ?
C16B C15B C14B 118.3(4) . . ?
C17B C16B C15B 120.6(4) . . ?
C16B C17B C18B 119.3(4) . . ?
C17B C18B C19B 118.9(4) . . ?
N2B C19B C18B 123.1(4) . . ?
N2B C19B C20B 115.0(3) . . ?
C18B C19B C20B 121.9(4) . . ?
N3B C20B C19B 115.4(4) . . ?
N3B C20B C21B 122.7(4) . . ?
C21B C20B C19B 121.9(4) . . ?
C22B C21B C20B 119.1(4) . . ?
C23B C22B C21B 118.7(4) . . ?
C22B C23B C24B 120.1(4) . . ?
N3B C24B C23B 121.8(4) . . ?
N3B C24B C25B 119.1(4) . . ?
C23B C24B C25B 118.9(4) . . ?
C26B C25B C24B 118.1(4) . . ?
C26B C25B C30B 120.3(4) . . ?
C30B C25B C24B 121.3(4) . . ?
C27B C26B C25B 121.4(5) . . ?
C28B C27B C26B 119.1(6) . . ?
C27B C28B C29B 120.7(5) . . ?
C28B C29B C30B 121.9(5) . . ?
C25B C30B C29B 116.6(5) . . ?
C25B C30B C31B 120.7(4) . . ?
C29B C30B C31B 122.7(5) . . ?
N4B C31B C30B 113.8(5) . . ?
N4B C33B C32B 116.2(9) . . ?
C35B C34B N4B 121.9(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1A Mn1A 2.5260(8) . ?
Mn1A N2A 2.071(4) . ?
Mn1A N3A 2.080(4) . ?
Mn1A C1A 1.819(5) . ?
Mn1A C2A 1.807(5) . ?
Mn1A C3A 1.809(4) . ?
O1A C2A 1.144(6) . ?
O2A C3A 1.146(5) . ?
O3A C1A 1.112(6) . ?
N1A C32A 1.376(9) . ?
N1A C34A 1.481(10) . ?
N1A C35A 1.517(10) . ?
N2A C20A 1.362(6) . ?
N2A C24A 1.355(6) . ?
N3A C15A 1.347(6) . ?
N3A C19A 1.352(6) . ?
N4A C5A 1.458(7) . ?
N4A C6A 1.463(6) . ?
N4A C8A 1.467(7) . ?
C4A C5A 1.503(8) . ?
C6A C7A 1.527(9) . ?
C8A C9A 1.503(8) . ?
C9A C10A 1.402(7) . ?
C9A C14A 1.394(7) . ?
C10A C11A 1.371(10) . ?
C11A C12A 1.401(11) . ?
C12A C13A 1.374(8) . ?
C13A C14A 1.400(7) . ?
C14A C15A 1.490(6) . ?
C15A C16A 1.398(7) . ?
C16A C17A 1.371(7) . ?
C17A C18A 1.380(7) . ?
C18A C19A 1.396(7) . ?
C19A C20A 1.460(7) . ?
C20A C21A 1.400(6) . ?
C21A C22A 1.381(7) . ?
C22A C23A 1.361(7) . ?
C23A C24A 1.398(6) . ?
C24A C25A 1.483(7) . ?
C25A C26A 1.389(7) . ?
C25A C30A 1.398(7) . ?
C26A C27A 1.390(7) . ?
C27A C28A 1.381(7) . ?
C28A C29A 1.386(8) . ?
C29A C30A 1.384(8) . ?
C30A C32A 1.526(8) . ?
C33A C34A 1.507(14) . ?
C35A C36A 1.552(11) . ?
Br1B Mn1B 2.5370(8) . ?
Mn1B N2B 2.068(3) . ?
Mn1B N3B 2.073(3) . ?
Mn1B C1B 1.796(5) . ?
Mn1B C2B 1.808(5) . ?
Mn1B C3B 1.815(5) . ?
O1B C1B 1.154(6) . ?
O2B C2B 1.147(6) . ?
O3B C3B 1.148(6) . ?
N1B C5B 1.432(8) . ?
N1B C6B 1.494(11) . ?
N1B C8B 1.437(7) . ?
N2B C15B 1.363(5) . ?
N2B C19B 1.363(5) . ?
N3B C20B 1.354(5) . ?
N3B C24B 1.360(5) . ?
N4B C31B 1.463(7) . ?
N4B C33B 1.463(9) . ?
N4B C34B 1.483(9) . ?
C4B C5B 1.551(12) . ?
C6B C7B 1.564(12) . ?
C8B C9B 1.523(8) . ?
C9B C10B 1.392(7) . ?
C9B C14B 1.409(6) . ?
C10B C11B 1.374(8) . ?
C11B C12B 1.372(8) . ?
C12B C13B 1.390(7) . ?
C13B C14B 1.388(6) . ?
C14B C15B 1.484(6) . ?
C15B C16B 1.408(6) . ?
C16B C17B 1.360(7) . ?
C17B C18B 1.379(6) . ?
C18B C19B 1.384(6) . ?
C19B C20B 1.474(5) . ?
C20B C21B 1.388(6) . ?
C21B C22B 1.383(6) . ?
C22B C23B 1.371(7) . ?
C23B C24B 1.388(6) . ?
C24B C25B 1.494(6) . ?
C25B C26B 1.398(7) . ?
C25B C30B 1.400(7) . ?
C26B C27B 1.373(7) . ?
C27B C28B 1.369(9) . ?
C28B C29B 1.376(9) . ?
C29B C30B 1.413(7) . ?
C30B C31B 1.522(8) . ?
C32B C33B 1.522(12) . ?
C34B C35B 1.387(11) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9998 4.9903 0.0022 -0.1150 -0.0250 0.0562
0.0010 -3.9903 4.9939 0.0448 0.2197 -0.0585
-4.9926 -1.0031 1.9943 0.0067 0.0934 0.2477
4.9926 1.0031 -1.9943 -0.0067 -0.0934 -0.2477
1.9982 -3.9880 4.9953 0.0438 0.2162 -0.1669
0.9998 -4.9925 -3.9991 0.1531 -0.1336 -0.0107
