#------------------------------------------------------------------------------
#$Date: 2019-05-14 03:54:13 +0300 (Tue, 14 May 2019) $
#$Revision: 215123 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/10/1551040.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_1551040
loop_
_publ_author_name
'Kadota, Kentaro'
'Duong, Nghia Tuan'
'Nishiyama, Yusuke'
'Sivaniah, Easan'
'Kitagawa, Susumu'
'Horike, Satoshi'
_publ_section_title
;
 Borohydride-containing coordination polymers: synthesis, air stability
 and dehydrogenation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00731H
_journal_year                    2019
_chemical_formula_sum            'C6.5 H11 B Mn0.5 N'
_chemical_formula_weight         141.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-07-13 deposited with the CCDC.    2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.764(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.155(3)
_cell_length_b                   13.178(7)
_cell_length_c                   11.242(6)
_cell_measurement_reflns_used    2265
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.4623
_cell_measurement_theta_min      3.0917
_cell_volume                     761.1(7)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6173
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         3.092
_exptl_absorpt_coefficient_mu    0.850
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       Rod
_exptl_crystal_F_000             298
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0464
_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)+(0.0285P)²+0.3819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1606
_reflns_number_total             1817
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc00731h2.cif
_cod_data_source_block           Mn-dpp
_cod_original_formula_sum        'C6.50 H11 B Mn0.50 N'
_cod_database_code               1551040
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.848
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Mn1 Mn -0.47534(9) 0.250000 0.27176(4) 0.02784(16) Uani 1 2 d S T P
N2 N -0.2531(3) 0.11031(13) 0.25571(15) 0.0272(4) Uani 1 1 d . . .
C11 C -0.1283(4) -0.03024(16) 0.1386(2) 0.0314(5) Uani 1 1 d . . .
H11 H -0.150(4) -0.0648(18) 0.068(2) 0.036(6) Uiso 1 1 d . . .
C12 C 0.0869(4) -0.00314(17) 0.3304(2) 0.0313(5) Uani 1 1 d . . .
C5 C -0.0730(4) 0.07976(16) 0.34188(19) 0.0304(5) Uani 1 1 d . . .
H5 H -0.060(4) 0.1204(18) 0.4096(19) 0.035(6) Uiso 1 1 d . . .
C6 C 0.0730(6) -0.250000 0.2379(3) 0.0285(6) Uani 1 2 d S T P
H6 H 0.033(6) -0.250000 0.320(3) 0.030(8) Uiso 1 2 d S . P
C7 C 0.0624(4) -0.06093(16) 0.22652(19) 0.0289(5) Uani 1 1 d . . .
C8 C -0.2767(4) 0.05400(17) 0.1554(2) 0.0314(5) Uani 1 1 d . . .
H8 H -0.399(4) 0.0772(17) 0.0961(19) 0.031(6) Uiso 1 1 d . . .
C9 C 0.2234(4) -0.15400(16) 0.2103(2) 0.0312(5) Uani 1 1 d . . .
H9 H 0.269(4) -0.1562(17) 0.127(2) 0.034(6) Uiso 1 1 d . . .
B1 B -0.7671(8) 0.250000 0.0983(3) 0.0318(8) Uani 1 2 d S T P
H17 H -0.755(4) 0.3188(17) 0.160(2) 0.041(7) Uiso 1 1 d . . .
B2 B -0.5605(9) 0.250000 0.4806(3) 0.0396(9) Uani 1 2 d S T P
H13 H -0.704(6) 0.250000 0.397(3) 0.028(8) Uiso 1 2 d S . P
H2 H -0.356(7) 0.250000 0.449(3) 0.054(11) Uiso 1 2 d S . P
H1 H 0.209(5) -0.0176(19) 0.393(2) 0.042(7) Uiso 1 1 d . . .
H16 H -0.956(7) 0.250000 0.046(3) 0.047(10) Uiso 1 2 d S . P
H15 H 0.380(4) -0.1489(17) 0.2601(19) 0.031(6) Uiso 1 1 d . . .
H14 H -0.091(6) -0.250000 0.194(3) 0.032(9) Uiso 1 2 d S . P
H18 H -0.596(8) 0.250000 0.046(3) 0.062(12) Uiso 1 2 d S . P
H19 H -0.587(6) 0.317(2) 0.527(3) 0.074(9) Uiso 1 1 d . . .
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'
B B 0.0013 0.0007 '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'
Mn Mn 0.3368 0.7283 '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'
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
N2 Mn1 N2 114.92(10) . 4_565
N2 Mn1 B1 103.55(7) . .
N2 Mn1 B1 103.55(7) 4_565 .
N2 Mn1 B2 102.62(7) . .
N2 Mn1 B2 102.62(7) 4_565 .
B1 Mn1 B2 130.22(15) . .
C5 N2 C8 116.52(19) . .
C5 N2 Mn1 121.85(14) . .
C8 N2 Mn1 121.47(14) . .
C8 C11 C7 120.4(2) . .
C5 C12 C7 119.9(2) . .
N2 C5 C12 123.4(2) . .
C9 C6 C9 111.7(3) . 4
C12 C7 C11 116.5(2) . .
C12 C7 C9 122.5(2) . .
C11 C7 C9 121.0(2) . .
N2 C8 C11 123.3(2) . .
C7 C9 C6 110.92(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N2 2.1836(19) .
Mn1 N2 2.184(2) 4_565
Mn1 B1 2.362(4) .
Mn1 B2 2.424(4) .
N2 C5 1.347(3) .
N2 C8 1.347(3) .
C11 C8 1.370(3) .
C11 C7 1.395(3) .
C12 C5 1.381(3) .
C12 C7 1.391(3) .
C6 C9 1.529(3) .
C6 C9 1.529(3) 4
C7 C9 1.500(3) .
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
C8 N2 C5 C12 1.4(3) .
Mn1 N2 C5 C12 -174.13(16) .
C7 C12 C5 N2 -1.3(3) .
C5 C12 C7 C11 -0.1(3) .
C5 C12 C7 C9 -177.7(2) .
C8 C11 C7 C12 1.3(3) .
C8 C11 C7 C9 178.9(2) .
C5 N2 C8 C11 -0.2(3) .
Mn1 N2 C8 C11 175.41(17) .
C7 C11 C8 N2 -1.2(3) .
C12 C7 C9 C6 97.5(3) .
C11 C7 C9 C6 -80.0(3) .
C9 C6 C9 C7 174.48(16) 4
