 
data_mo-ba_400_mn_a
 
_audit_creation_method            'SHELXL-2019/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C4 H11 Br Mn0.80 N Pb0.70'
_chemical_formula_sum
 'C4 H11 Br Mn0.80 N Pb0.70' 
_chemical_formula_weight          342.03

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'
 'Pb'  'Pb'  -3.3944  10.1111
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            61
_space_group_name_H-M_alt         'P b c a'
_space_group_name_Hall            '-P 2ac 2ab'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    8.2611(9)
_cell_length_b                    8.1366(9)
_cell_length_c                    27.461(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1845.9(4)
_cell_formula_units_Z             8
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     5916
_cell_measurement_theta_min       2.878
_cell_measurement_theta_max      30.566
 
_exptl_crystal_description        'prism frag'
_exptl_crystal_colour             'colorless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.462          
_exptl_crystal_F_000              1235
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.291
_exptl_crystal_size_mid           0.254
_exptl_crystal_size_min           0.086
_exptl_absorpt_coefficient_mu     18.124
_shelx_estimated_absorpt_T_min    0.077
_shelx_estimated_absorpt_T_max    0.305
_exptl_absorpt_correction_type   'multi-scan'
_exptl_absorpt_correction_T_min   0.077
_exptl_absorpt_correction_T_max    0.305
_exptl_absorpt_process_details   'Sadabs'
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker AXS D8 Venture'
_diffrn_measurement_method        'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             53748
_diffrn_reflns_av_unetI/netI      0.0291
_diffrn_reflns_av_R_equivalents   0.0662
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -39
_diffrn_reflns_limit_l_max        39
_diffrn_reflns_theta_min          2.878
_diffrn_reflns_theta_max          30.566
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.994
_diffrn_measured_fraction_theta_full  0.994
_diffrn_reflns_Laue_measured_fraction_max    0.994
_diffrn_reflns_Laue_measured_fraction_full   0.994
_diffrn_reflns_point_group_measured_fraction_max   0.994
_diffrn_reflns_point_group_measured_fraction_full  0.994
_reflns_number_total              2817
_reflns_number_gt                 2598
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.Electronic residual 
 Densities remained at the vicinity of the Pb and Br atoms. All attempts
 to fit them in any reasonable chemically model failed.
;
 
_computing_data_collection 'APEX5 v2023.9.2'
_computing_cell_refinement 'APEX5 v2023.9.2'
_computing_data_reduction  'Saint, APEX5 v2023.9.2.'
_computing_structure_solution 'SHELXT'
_computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics  'Mercury 2022-3.0,POV-Ray v 3.7'
_computing_publication_material 'APEX5 v2023.9.2'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1546P)²+39.6749P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2817
_refine_ls_number_parameters      76
_refine_ls_number_restraints      12
_refine_ls_R_factor_all           0.0919
_refine_ls_R_factor_gt            0.0876
_refine_ls_wR_factor_ref          0.2757
_refine_ls_wR_factor_gt           0.2705
_refine_ls_goodness_of_fit_ref    1.306
_refine_ls_restrained_S_all       1.305
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
Pb1 Pb 0.500000 1.000000 0.500000 0.0113(3) Uani 1 2 d S . P . .
Mn1 Mn 0.305(4) 0.696(3) 0.4993(8) 0.0166(12) Uani 0.8 1 d . . P A 1
Pb2 Pb 0.313(3) 0.684(3) 0.4979(7) 0.0166(12) Uani 0.2 1 d . . P A 2
Br1 Br 0.46897(18) 1.01812(14) 0.60931(5) 0.0175(3) Uani 1 1 d . . . . .
N1 N 0.4262(11) 0.4223(12) 0.5891(4) 0.0180(17) Uani 1 1 d . . . . .
H1U H 0.357010 0.364260 0.606389 0.022 Uiso 1 1 calc R U . . .
H1V H 0.426112 0.414825 0.557155 0.022 Uiso 1 1 calc R U . . .
C2 C 0.5185(15) 0.5235(15) 0.6696(5) 0.017(2) Uani 1 1 d . U . . .
H2A H 0.406054 0.555512 0.677681 0.020 Uiso 1 1 calc R U . . .
H2B H 0.535364 0.408966 0.680723 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6378(15) 0.6382(18) 0.6961(5) 0.029(3) Uani 1 1 d . . . . .
H3A H 0.749759 0.609216 0.686567 0.034 Uiso 1 1 calc R U . . .
H3B H 0.617519 0.752953 0.685787 0.034 Uiso 1 1 calc R U . . .
C1 C 0.5440(13) 0.5335(15) 0.6141(4) 0.019(2) Uani 1 1 d . U . . .
H1A H 0.527744 0.648015 0.602930 0.022 Uiso 1 1 calc R U . . .
H1B H 0.656046 0.500348 0.605912 0.022 Uiso 1 1 calc R U . . .
C4 C 0.622(2) 0.627(3) 0.7505(5) 0.051(5) Uani 1 1 d . . . . .
H4A H 0.507671 0.625984 0.759534 0.076 Uiso 1 1 calc R U . . .
H4B H 0.675516 0.722062 0.765553 0.076 Uiso 1 1 calc R U . . .
H4C H 0.674152 0.525755 0.761974 0.076 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Pb1 Mn1 2.95(3) . ?
Pb1 Mn1 2.95(3) 5_676 ?
Pb1 Mn1 2.98(3) 8_665 ?
Pb1 Mn1 2.98(3) 4_566 ?
Pb1 Pb2 2.99(3) 8_665 ?
Pb1 Pb2 2.99(3) 4_566 ?
Pb1 Pb2 3.00(3) 5_676 ?
Pb1 Pb2 3.00(3) . ?
Pb1 Br1 3.0164(13) . ?
Pb1 Br1 3.0165(13) 5_676 ?
N1 C1 1.496(14) . ?
N1 H1U 0.8800 . ?
N1 H1V 0.8800 . ?
C2 C3 1.540(17) . ?
C2 C1 1.541(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.502(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
 
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
Mn1 Pb1 Mn1 180.0 . 5_676 ?
Mn1 Pb1 Mn1 89.2(2) . 8_665 ?
Mn1 Pb1 Mn1 90.8(2) 5_676 8_665 ?
Mn1 Pb1 Mn1 90.8(2) . 4_566 ?
Mn1 Pb1 Mn1 89.2(2) 5_676 4_566 ?
Mn1 Pb1 Mn1 180.0 8_665 4_566 ?
Mn1 Pb1 Pb2 87.0(11) . 8_665 ?
Mn1 Pb1 Pb2 93.0(11) 5_676 8_665 ?
Mn1 Pb1 Pb2 2.4(10) 8_665 8_665 ?
Mn1 Pb1 Pb2 177.6(10) 4_566 8_665 ?
Mn1 Pb1 Pb2 93.0(11) . 4_566 ?
Mn1 Pb1 Pb2 87.0(11) 5_676 4_566 ?
Mn1 Pb1 Pb2 177.6(10) 8_665 4_566 ?
Mn1 Pb1 Pb2 2.4(10) 4_566 4_566 ?
Mn1 Pb1 Pb2 177.8(11) . 5_676 ?
Mn1 Pb1 Pb2 2.2(11) 5_676 5_676 ?
Mn1 Pb1 Pb2 88.7(11) 8_665 5_676 ?
Mn1 Pb1 Pb2 91.3(11) 4_566 5_676 ?
Pb2 Pb1 Pb2 89.1(3) 8_665 . ?
Pb2 Pb1 Pb2 90.9(3) 4_566 . ?
Pb2 Pb1 Pb2 180.0 5_676 . ?
Mn1 Pb1 Br1 90.0(4) . . ?
Mn1 Pb1 Br1 90.0(4) 5_676 . ?
Mn1 Pb1 Br1 84.7(4) 8_665 . ?
Mn1 Pb1 Br1 95.3(4) 4_566 . ?
Pb2 Pb1 Br1 85.5(4) 8_665 . ?
Pb2 Pb1 Br1 94.5(4) 4_566 . ?
Pb2 Pb1 Br1 89.0(4) 5_676 . ?
Pb2 Pb1 Br1 91.0(4) . . ?
Mn1 Pb1 Br1 90.0(4) . 5_676 ?
Mn1 Pb1 Br1 90.0(4) 5_676 5_676 ?
Mn1 Pb1 Br1 95.3(4) 8_665 5_676 ?
Mn1 Pb1 Br1 84.7(4) 4_566 5_676 ?
Pb2 Pb1 Br1 94.5(4) 8_665 5_676 ?
Pb2 Pb1 Br1 85.5(4) 4_566 5_676 ?
Pb2 Pb1 Br1 91.0(4) 5_676 5_676 ?
Pb2 Pb1 Br1 89.0(4) . 5_676 ?
Br1 Pb1 Br1 180.0 . 5_676 ?
Pb1 Mn1 Pb1 155.4(11) . 4_466 ?
Pb1 Pb2 Pb1 150.9(10) 4_466 . ?
C1 N1 H1U 120.0 . . ?
C1 N1 H1V 120.0 . . ?
H1U N1 H1V 120.0 . . ?
C3 C2 C1 110.3(10) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 112.3(13) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
N1 C1 C2 109.4(9) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C1 C2 C3 C4 -177.5(12) . . . . ?
C3 C2 C1 N1 -179.6(10) . . . . ?
 
_refine_diff_density_max    6.092
_refine_diff_density_min   -6.184
_refine_diff_density_rms    0.961



