data_3AMP
_audit_creation_date               2020-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'Br4 Mn, H2 O, C6 H16 N2'
_chemical_formula_sum              'C6 H18 Br4 Mn N2 O'
_chemical_formula_weight           508.80
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
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'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             4
_space_group_name_H-M_alt          'P 1 21 1'
_space_group_name_Hall             'P 2yb'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'

_cell_length_a                     8.481(8)
_cell_length_b                     8.547(7)
_cell_length_c                     10.645(9)
_cell_angle_alpha                  90
_cell_angle_beta                   108.72(3)
_cell_angle_gamma                  90
_cell_volume                       730.8(11)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      1587
_cell_measurement_temperature      300(2)
_cell_measurement_theta_max        25.26
_cell_measurement_theta_min        2.54
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      11.815
_exptl_absorpt_correction_T_max    ?
_exptl_absorpt_correction_T_min    ?
_exptl_absorpt_correction_type     'none'
_exptl_absorpt_process_details     ?
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'pale yellow'
_exptl_crystal_density_diffrn      2.312
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               482
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0488
_diffrn_reflns_av_unetI/netI       0.1052
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.991
_diffrn_reflns_limit_h_max         5
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         11
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         14
_diffrn_reflns_limit_l_min         -13
_diffrn_reflns_number              5563
_diffrn_reflns_point_group_measured_fraction_full  0.960
_diffrn_reflns_point_group_measured_fraction_max  0.930
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           28.440
_diffrn_reflns_theta_min           2.020
_diffrn_ambient_temperature        299.7
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.991
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.761
_reflns_Friedel_fraction_full      0.914
_reflns_Friedel_fraction_max       0.861
_reflns_number_gt                  2461
_reflns_number_total               3426
_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.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      'XT (Sheldrick, 2015)'
_refine_diff_density_max           0.867
_refine_diff_density_min           -1.191
_refine_diff_density_rms           0.173
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack     0.00(3)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     0.937
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       131
_refine_ls_number_reflns           3426
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0745
_refine_ls_R_factor_gt             0.0527
_refine_ls_restrained_S_all        0.937
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0532P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1155
_refine_ls_wR_factor_ref           0.1237
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O006(H00N,H00O)
2.b Ternary CH refined with riding coordinates:
 C00B(H00G)
2.c Secondary CH2 refined with riding coordinates:
 N007(H00A,H00B), C009(H00C,H00D), C00A(H00E,H00F), C00C(H00H,H00I), C00D(H00J,
 H00K), C00E(H00L,H00M)
2.d Idealised Me refined as rotating group:
 N8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
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
 Br01 Br 0.21827(16) 0.20452(17) 0.54827(14) 0.0345(3) Uani 1 1 d . . . . .
 Br02 Br 0.60010(14) 0.50226(17) 0.72531(15) 0.0362(4) Uani 1 1 d . . . . .
 Br03 Br 0.13380(14) 0.51618(17) 0.79020(15) 0.0370(4) Uani 1 1 d . . . . .
 Br04 Br 0.45425(17) 0.15714(18) 0.94025(14) 0.0389(4) Uani 1 1 d . . . . .
 Mn05 Mn 0.3635(2) 0.3542(2) 0.7584(2) 0.0278(5) Uani 1 1 d . . . . .
 O006 O 0.3129(12) 0.8416(13) 0.7231(10) 0.038(2) Uani 1 1 d . . . . .
 H00N H 0.2551 0.7773 0.7542 0.057 Uiso 1 1 d G . . . .
 H00O H 0.3365 0.9248 0.7727 0.057 Uiso 1 1 d G . . . .
 N007 N 0.3085(12) 0.3896(14) 0.1666(12) 0.034(3) Uani 1 1 d . . . . .
 H00A H 0.3806 0.3086 0.1743 0.041 Uiso 1 1 calc R . . . .
 H00B H 0.3279 0.4604 0.1094 0.041 Uiso 1 1 calc R . . . .
 N8 N 0.1742(13) 0.8064(13) 0.4432(12) 0.036(3) Uani 1 1 d . . . . .
 H8A H 0.2054 0.8813 0.3952 0.043 Uiso 1 1 calc GR . . . .
 H8B H 0.2028 0.8370 0.5295 0.043 Uiso 1 1 calc GR . . . .
 H8C H 0.0621 0.7922 0.4103 0.043 Uiso 1 1 calc GR . . . .
 C009 C 0.1340(16) 0.3299(16) 0.1101(16) 0.038(4) Uani 1 1 d . . . . .
 H00C H 0.1167 0.2871 0.0202 0.046 Uiso 1 1 calc R . . . .
 H00D H 0.1157 0.2444 0.1666 0.046 Uiso 1 1 calc R . . . .
 C00A C 0.0411(13) 0.5354(17) 0.2375(14) 0.034(3) Uani 1 1 d . . . . .
 H00E H 0.0186 0.4584 0.2992 0.041 Uiso 1 1 calc R . . . .
 H00F H -0.0371 0.6239 0.2281 0.041 Uiso 1 1 calc R . . . .
 C00B C 0.2202(14) 0.5949(16) 0.2950(14) 0.028(3) Uani 1 1 d . . . . .
 H00G H 0.2376 0.6807 0.2369 0.034 Uiso 1 1 calc R . . . .
 C00C C 0.2602(15) 0.6566(17) 0.4344(13) 0.034(3) Uani 1 1 d . . . . .
 H00H H 0.2284 0.5769 0.4893 0.041 Uiso 1 1 calc R . . . .
 H00I H 0.3819 0.6728 0.4720 0.041 Uiso 1 1 calc R . . . .
 C00D C 0.0124(16) 0.4590(19) 0.1028(16) 0.043(4) Uani 1 1 d . . . . .
 H00J H -0.1022 0.4165 0.0701 0.051 Uiso 1 1 calc R . . . .
 H00K H 0.0231 0.5389 0.0387 0.051 Uiso 1 1 calc R . . . .
 C00E C 0.3415(15) 0.4646(17) 0.2983(15) 0.034(3) Uani 1 1 d . . . . .
 H00L H 0.4562 0.5072 0.3281 0.040 Uiso 1 1 calc R . . . .
 H00M H 0.3340 0.3847 0.3635 0.040 Uiso 1 1 calc R . . . .


_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
 Br01 Mn05 2.528(3) . ?
 Br02 Mn05 2.491(3) . ?
 Br03 Mn05 2.500(3) . ?
 Br04 Mn05 2.495(3) . ?
 O006 H00N 0.8699 . ?
 O006 H00O 0.8700 . ?
 N007 H00A 0.9100 . ?
 N007 H00B 0.9100 . ?
 N007 C009 1.496(16) . ?
 N007 C00E 1.485(18) . ?
 N8 H8A 0.9100 . ?
 N8 H8B 0.9100 . ?
 N8 H8C 0.9100 . ?
 N8 C00C 1.491(17) . ?
 C009 H00C 0.9900 . ?
 C009 H00D 0.9900 . ?
 C009 C00D 1.50(2) . ?
 C00A H00E 0.9900 . ?
 C00A H00F 0.9900 . ?
 C00A C00B 1.531(16) . ?
 C00A C00D 1.52(2) . ?
 C00B H00G 1.0000 . ?
 C00B C00C 1.508(19) . ?
 C00B C00E 1.509(17) . ?
 C00C H00H 0.9900 . ?
 C00C H00I 0.9900 . ?
 C00D H00J 0.9900 . ?
 C00D H00K 0.9900 . ?
 C00E H00L 0.9900 . ?
 C00E H00M 0.9900 . ?

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
 Br02 Mn05 Br01 108.55(10) . . ?
 Br02 Mn05 Br03 115.86(11) . . ?
 Br02 Mn05 Br04 113.01(9) . . ?
 Br03 Mn05 Br01 102.74(9) . . ?
 Br04 Mn05 Br01 106.63(11) . . ?
 Br04 Mn05 Br03 109.17(10) . . ?
 H00N O006 H00O 109.5 . . ?
 H00A N007 H00B 107.8 . . ?
 C009 N007 H00A 109.0 . . ?
 C009 N007 H00B 109.0 . . ?
 C00E N007 H00A 109.0 . . ?
 C00E N007 H00B 109.0 . . ?
 C00E N007 C009 112.9(11) . . ?
 H8A N8 H8B 109.5 . . ?
 H8A N8 H8C 109.5 . . ?
 H8B N8 H8C 109.5 . . ?
 C00C N8 H8A 109.5 . . ?
 C00C N8 H8B 109.5 . . ?
 C00C N8 H8C 109.5 . . ?
 N007 C009 H00C 109.6 . . ?
 N007 C009 H00D 109.6 . . ?
 H00C C009 H00D 108.1 . . ?
 C00D C009 N007 110.2(11) . . ?
 C00D C009 H00C 109.6 . . ?
 C00D C009 H00D 109.6 . . ?
 H00E C00A H00F 108.0 . . ?
 C00B C00A H00E 109.5 . . ?
 C00B C00A H00F 109.5 . . ?
 C00D C00A H00E 109.5 . . ?
 C00D C00A H00F 109.5 . . ?
 C00D C00A C00B 110.9(11) . . ?
 C00A C00B H00G 108.7 . . ?
 C00C C00B C00A 113.0(11) . . ?
 C00C C00B H00G 108.7 . . ?
 C00C C00B C00E 107.4(10) . . ?
 C00E C00B C00A 110.2(11) . . ?
 C00E C00B H00G 108.7 . . ?
 N8 C00C C00B 113.7(11) . . ?
 N8 C00C H00H 108.8 . . ?
 N8 C00C H00I 108.8 . . ?
 C00B C00C H00H 108.8 . . ?
 C00B C00C H00I 108.8 . . ?
 H00H C00C H00I 107.7 . . ?
 C009 C00D C00A 111.6(12) . . ?
 C009 C00D H00J 109.3 . . ?
 C009 C00D H00K 109.3 . . ?
 C00A C00D H00J 109.3 . . ?
 C00A C00D H00K 109.3 . . ?
 H00J C00D H00K 108.0 . . ?
 N007 C00E C00B 112.1(11) . . ?
 N007 C00E H00L 109.2 . . ?
 N007 C00E H00M 109.2 . . ?
 C00B C00E H00L 109.2 . . ?
 C00B C00E H00M 109.2 . . ?
 H00L C00E H00M 107.9 . . ?

_olex2_submission_special_instructions  'No special instructions were received'
