 
data_P21
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'Br3 Mn, C4 H9 F N'
_chemical_formula_sum
 'C4 H9 Br3 F Mn N' 
_chemical_formula_weight          384.76

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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            4
_space_group_name_H-M_alt         'P 21'
_space_group_name_Hall            'P 2yb'
 
_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, y+1/2, -z'
 
_cell_length_a                    7.8558(4)
_cell_length_b                    6.7422(3)
_cell_length_c                    9.7844(5)
_cell_angle_alpha                 90
_cell_angle_beta                  113.669(3)
_cell_angle_gamma                 90
_cell_volume                      474.64(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     223(2)
_cell_measurement_reflns_used     3447
_cell_measurement_theta_min       2.8200
_cell_measurement_theta_max       30.3300
 
_exptl_crystal_description        Prism
_exptl_crystal_colour             Red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.692          
_exptl_crystal_F_000              358
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.210
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.200
_exptl_absorpt_coefficient_mu     13.965
_shelx_estimated_absorpt_T_min    0.157
_shelx_estimated_absorpt_T_max    0.167
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.061
_exptl_absorpt_correction_T_max   0.075
_exptl_absorpt_process_details    'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       223(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Rotating-anode X-ray tube'
_diffrn_measurement_device_type   'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method        'four-circle diffractometer'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             5357
_diffrn_reflns_av_unetI/netI      0.0665
_diffrn_reflns_av_R_equivalents   0.0899
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          2.831
_diffrn_reflns_theta_max          24.981
_diffrn_reflns_theta_full         24.981
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              1661
_reflns_number_gt                 1462
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.829
_reflns_Friedel_fraction_max      1.000
_reflns_Friedel_fraction_full     1.000
 
_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.
;
 
_computing_data_collection        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution     'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material   'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1233P)²+6.5174P] 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_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.39(6)
_chemical_absolute_configuration  rm
_refine_ls_number_reflns          1661
_refine_ls_number_parameters      92
_refine_ls_number_restraints      44
_refine_ls_R_factor_all           0.0802
_refine_ls_R_factor_gt            0.0737
_refine_ls_wR_factor_ref          0.1968
_refine_ls_wR_factor_gt           0.1914
_refine_ls_goodness_of_fit_ref    1.003
_refine_ls_restrained_S_all       0.994
_refine_ls_shift/su_max           0.003
_refine_ls_shift/su_mean          0.001
 
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
Mn1 Mn 0.9967(4) 1.0018(4) 1.0015(4) 0.0285(4) Uani 1 1 d . . . . .
Br1 Br 1.17810(13) 0.7513(3) 0.88610(11) 0.0357(2) Uani 1 1 d . . . . .
Br2 Br 1.11878(14) 0.7462(3) 1.23681(11) 0.0373(3) Uani 1 1 d . . . . .
Br3 Br 0.70912(12) 0.7515(3) 0.89136(12) 0.0360(3) Uani 1 1 d . . . . .
N1 N 0.3608(16) 0.1459(10) 0.7678(8) 0.047(3) Uani 1 1 d D U . . .
H1A H 0.4601 0.0909 0.8409 0.056 Uiso 1 1 calc R U . . .
H1B H 0.2621 0.1339 0.7920 0.056 Uiso 1 1 calc R U . . .
C1 C 0.323(2) 0.0449(13) 0.6225(7) 0.070(5) Uani 1 1 d D U . . .
H1C H 0.2264 -0.0563 0.6022 0.084 Uiso 1 1 calc R U . . .
H1D H 0.4359 -0.0186 0.6240 0.084 Uiso 1 1 calc R U . . .
C2 C 0.2592(11) 0.2054(11) 0.5066(8) 0.084(5) Uani 1 1 d D U . . .
H2 H 0.1413 0.1810 0.4192 0.101 Uiso 1 1 calc R U . . .
C3 C 0.273(3) 0.3970(14) 0.5891(9) 0.095(6) Uani 1 1 d D U . . .
H3A H 0.3245 0.5015 0.5475 0.115 Uiso 1 1 calc R U . . .
H3B H 0.1494 0.4389 0.5804 0.115 Uiso 1 1 calc R U . . .
F1 F 0.4149(10) 0.198(3) 0.4826(12) 0.202(9) Uani 1 1 d D U . . .
C4 C 0.3975(16) 0.3605(11) 0.7495(9) 0.036(3) Uani 1 1 d D U . . .
H4A H 0.3639 0.4450 0.8163 0.043 Uiso 1 1 calc R U . . .
H4B H 0.5282 0.3829 0.7680 0.043 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
Mn1 Br1 2.672(4) 2_757 ?
Mn1 Br3 2.676(3) . ?
Mn1 Br2 2.697(3) 2_757 ?
Mn1 Br3 2.707(3) 2_757 ?
Mn1 Br2 2.724(3) . ?
Mn1 Br1 2.729(4) . ?
Br1 Mn1 2.672(4) 2_747 ?
Br2 Mn1 2.697(3) 2_747 ?
Br3 Mn1 2.707(3) 2_747 ?
N1 C1 1.495(9) . ?
N1 C4 1.500(9) . ?
C1 C2 1.500(9) . ?
C2 F1 1.336(10) . ?
C2 C3 1.504(10) . ?
C3 C4 1.499(9) . ?
 
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
Br1 Mn1 Br3 94.15(10) 2_757 . ?
Br1 Mn1 Br2 85.48(9) 2_757 2_757 ?
Br3 Mn1 Br2 95.77(10) . 2_757 ?
Br1 Mn1 Br3 87.08(10) 2_757 2_757 ?
Br3 Mn1 Br3 178.70(16) . 2_757 ?
Br2 Mn1 Br3 83.89(10) 2_757 2_757 ?
Br1 Mn1 Br2 96.60(12) 2_757 . ?
Br3 Mn1 Br2 83.98(10) . . ?
Br2 Mn1 Br2 177.91(15) 2_757 . ?
Br3 Mn1 Br2 96.31(9) 2_757 . ?
Br1 Mn1 Br1 179.20(15) 2_757 . ?
Br3 Mn1 Br1 86.54(10) . . ?
Br2 Mn1 Br1 94.06(12) 2_757 . ?
Br3 Mn1 Br1 92.23(10) 2_757 . ?
Br2 Mn1 Br1 83.86(9) . . ?
Mn1 Br1 Mn1 77.25(3) 2_747 . ?
Mn1 Br2 Mn1 76.92(3) 2_747 . ?
Mn1 Br3 Mn1 77.57(2) . 2_747 ?
C1 N1 C4 107.4(7) . . ?
N1 C1 C2 105.6(7) . . ?
F1 C2 C1 93.1(10) . . ?
F1 C2 C3 104.7(14) . . ?
C1 C2 C3 106.5(7) . . ?
C4 C3 C2 107.2(7) . . ?
C3 C4 N1 102.0(7) . . ?
 
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
C4 N1 C1 C2 -23.2(13) . . . . ?
N1 C1 C2 F1 109.7(12) . . . . ?
N1 C1 C2 C3 3.3(15) . . . . ?
F1 C2 C3 C4 -80.2(14) . . . . ?
C1 C2 C3 C4 17.6(16) . . . . ?
C2 C3 C4 N1 -31.0(16) . . . . ?
C1 N1 C4 C3 33.4(14) . . . . ?
 
_refine_diff_density_max    1.508
_refine_diff_density_min   -1.180
_refine_diff_density_rms    0.255



