#------------------------------------------------------------------------------
#$Date: 2019-05-14 03:54:13 +0300 (Tue, 14 May 2019) $
#$Revision: 215123 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/10/1551043.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_1551043
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            'C22 H30 B2 Mn N5'
_chemical_formula_weight         441.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                103.895(5)
_cell_angle_beta                 99.016(5)
_cell_angle_gamma                98.093(5)
_cell_formula_units_Z            2
_cell_length_a                   9.794(5)
_cell_length_b                   10.087(5)
_cell_length_c                   12.178(5)
_cell_measurement_reflns_used    2470
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.4507
_cell_measurement_theta_min      3.0297
_cell_volume                     1133.3(9)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_unetI/netI     0.1728
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9277
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         3.158
_exptl_absorpt_coefficient_mu    0.601
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       Rod
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.0916
_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)+(0.0521P)²+0.9451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2588
_reflns_number_total             4954
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9sc00731h2.cif
_cod_data_source_block           Mnbib
_cod_database_code               1551043
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Mn1 Mn 0.45681(9) 0.23338(9) 0.76470(7) 0.0292(3) Uani 1 1 d . .
N2 N 0.3655(5) 0.3260(5) 0.4314(4) 0.0266(10) Uani 1 1 d . .
N3 N 0.4000(5) 0.3096(5) 0.6090(4) 0.0293(11) Uani 1 1 d . .
N4 N 0.5387(5) 0.1741(4) 0.9241(3) 0.0258(10) Uani 1 1 d . .
N7 N 0.6897(5) 0.0915(4) 1.0343(4) 0.0264(10) Uani 1 1 d . .
N5 N 0.8843(5) 0.2988(5) 0.7009(4) 0.0281(11) Uani 1 1 d . .
C7 C 0.7980(6) 0.3567(6) 0.8563(5) 0.0328(14) Uani 1 1 d . .
C8 C 1.0323(6) 0.5317(6) 0.6173(4) 0.0288(13) Uani 1 1 d . .
H48 H 1.054302 0.554823 0.699213 0.035 Uiso 1 1 calc R U
C9 C -0.0699(5) 0.0802(5) 0.1286(4) 0.0240(12) Uani 1 1 d . .
C10 C 0.9213(7) 0.3529(6) 0.8186(5) 0.0328(14) Uani 1 1 d . .
C11 C 0.3290(6) 0.4408(6) 0.4958(5) 0.0327(14) Uani 1 1 d . .
H49 H 0.295030 0.513710 0.469523 0.039 Uiso 1 1 calc R U
N6 N 0.6859(5) 0.3040(5) 0.7652(4) 0.0285(11) Uani 1 1 d . .
C13 C 0.1279(6) 0.2668(6) 0.1644(5) 0.0297(13) Uani 1 1 d . .
C14 C 0.7421(6) 0.2715(6) 0.6740(5) 0.0313(14) Uani 1 1 d . .
C15 C 0.3530(7) 0.2843(7) 0.3063(5) 0.0347(15) Uani 1 1 d . .
H15 H 0.421(6) 0.232(6) 0.294(4) 0.036(17) Uiso 1 1 d . .
C16 C 0.1427(6) 0.0915(6) 0.2633(5) 0.0318(14) Uani 1 1 d . .
C25 C 0.6203(6) 0.0818(6) 0.9260(5) 0.0306(14) Uani 1 1 d . .
H43 H 0.637(5) 0.022(5) 0.872(4) 0.025(15) Uiso 1 1 d . .
B18 B 0.3075(8) 0.3807(8) 0.8720(6) 0.0375(18) Uani 1 1 d . .
H27 H 0.258(5) 0.262(5) 0.801(4) 0.035(15) Uiso 1 1 d . .
C26 C 0.6465(7) 0.1977(6) 1.1049(5) 0.0377(16) Uani 1 1 d . .
C17 C 0.3513(6) 0.4291(7) 0.6050(5) 0.0313(14) Uani 1 1 d . .
H17 H 0.346(5) 0.482(5) 0.665(4) 0.022(15) Uiso 1 1 d . .
C19 C -0.0072(6) 0.1998(6) 0.1059(5) 0.0287(13) Uani 1 1 d . .
H19 H -0.068(7) 0.233(6) 0.048(5) 0.06(2) Uiso 1 1 d . .
C20 C 0.2048(6) 0.2139(5) 0.2432(4) 0.0262(12) Uani 1 1 d . .
C22 C 0.9880(5) 0.3950(6) 0.5569(5) 0.0266(12) Uani 1 1 d . .
C23 C 0.9780(7) 0.2789(7) 0.6170(6) 0.0335(15) Uani 1 1 d . .
C18 C 0.4072(6) 0.2503(6) 0.5021(5) 0.0331(14) Uani 1 1 d . .
H18 H 0.446(6) 0.161(6) 0.477(4) 0.039(16) Uiso 1 1 d . .
B26 B 0.3741(9) -0.0175(8) 0.6413(6) 0.0345(16) Uani 1 1 d . .
H31 H 0.378(6) -0.111(6) 0.654(5) 0.047(17) Uiso 1 1 d . .
C21 C 0.0072(7) 0.0255(6) 0.2065(5) 0.0348(15) Uani 1 1 d . .
C24 C 1.0460(6) 0.6373(6) 0.5630(5) 0.0315(14) Uani 1 1 d . .
H24 H 1.064(5) 0.722(4) 0.600(3) 0.003(11) Uiso 1 1 d . .
C27 C 0.5569(6) 0.2480(6) 1.0369(5) 0.0290(13) Uani 1 1 d . .
C28 C 0.7834(7) 0.0019(6) 1.0662(6) 0.0341(14) Uani 1 1 d . .
H46 H 0.788(6) -0.062(5) 1.001(5) 0.029(16) Uiso 1 1 d . .
H1 H 0.426(5) 0.407(4) 0.860(4) 0.020(13) Uiso 1 1 d . .
H28 H 0.485(6) 0.054(5) 0.661(4) 0.031(14) Uiso 1 1 d . .
H36 H 0.678(5) 0.221(4) 1.177(4) 0.009(12) Uiso 1 1 d . .
H25 H 0.258(6) 0.453(6) 0.839(5) 0.044(17) Uiso 1 1 d . .
H37 H 0.504(5) 0.307(5) 1.054(4) 0.023(15) Uiso 1 1 d . .
H29 H 0.319(5) 0.050(5) 0.699(4) 0.034(15) Uiso 1 1 d . .
H30 H 0.329(6) -0.022(6) 0.563(5) 0.051(19) Uiso 1 1 d . .
H38 H 0.705(5) 0.227(5) 0.598(4) 0.021(14) Uiso 1 1 d . .
H39 H 1.007(6) 0.378(6) 0.848(5) 0.034(17) Uiso 1 1 d . .
H35 H 0.165(6) 0.345(5) 0.149(4) 0.035(16) Uiso 1 1 d . .
H32 H 0.192(7) 0.061(6) 0.323(5) 0.054(19) Uiso 1 1 d . .
H40 H 0.950(6) 0.182(6) 0.564(5) 0.045(18) Uiso 1 1 d . .
H41 H 1.057(7) 0.278(6) 0.652(5) 0.04(2) Uiso 1 1 d . .
H26 H 0.296(6) 0.374(5) 0.951(5) 0.046(17) Uiso 1 1 d . .
H33 H -0.031(5) -0.051(5) 0.220(4) 0.021(14) Uiso 1 1 d . .
H34 H 0.376(6) 0.367(5) 0.286(4) 0.030(16) Uiso 1 1 d . .
H45 H 0.792(7) 0.388(6) 0.930(5) 0.06(2) Uiso 1 1 d . .
H47 H 0.732(8) -0.048(7) 1.107(6) 0.09(3) 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
N4 Mn1 N3 173.07(17) . .
N4 Mn1 N6 84.53(16) . .
N3 Mn1 N6 88.97(16) . .
N4 Mn1 B18 90.4(2) . .
N3 Mn1 B18 91.3(2) . .
N6 Mn1 B18 124.6(2) . .
N4 Mn1 B26 94.4(2) . .
N3 Mn1 B26 90.0(2) . .
N6 Mn1 B26 109.9(2) . .
B18 Mn1 B26 125.5(3) . .
C18 N2 C11 107.9(5) . .
C18 N2 C15 124.6(5) . .
C11 N2 C15 127.4(5) . .
C18 N3 C17 105.2(5) . .
C18 N3 Mn1 127.6(4) . .
C17 N3 Mn1 127.2(4) . .
C25 N4 C27 104.5(5) . .
C25 N4 Mn1 123.3(4) . .
C27 N4 Mn1 129.0(4) . .
C25 N7 C26 105.3(5) . .
C25 N7 C28 126.3(5) . .
C26 N7 C28 128.3(5) . .
C14 N5 C10 106.7(5) . .
C14 N5 C23 125.3(5) . .
C10 N5 C23 128.0(5) . .
C10 C7 N6 110.4(5) . .
C22 C8 C24 122.2(5) . .
C19 C9 C21 118.5(5) . .
C19 C9 C28 122.6(5) . 1_454
C21 C9 C28 118.8(5) . 1_454
C7 C10 N5 105.7(5) . .
C17 C11 N2 105.3(5) . .
C14 N6 C7 105.1(5) . .
C14 N6 Mn1 123.4(4) . .
C7 N6 Mn1 129.9(4) . .
C20 C13 C19 121.4(5) . .
N6 C14 N5 112.2(5) . .
N2 C15 C20 112.6(5) . .
C21 C16 C20 120.9(5) . .
N4 C25 N7 112.6(5) . .
C27 C26 N7 107.0(5) . .
C11 C17 N3 110.4(5) . .
C9 C19 C13 120.4(5) . .
C13 C20 C16 117.9(5) . .
C13 C20 C15 122.1(5) . .
C16 C20 C15 120.0(5) . .
C8 C22 C24 118.3(5) . 2_766
C8 C22 C23 121.9(5) . .
C24 C22 C23 119.8(5) 2_766 .
N5 C23 C22 111.6(5) . .
N3 C18 N2 111.2(5) . .
C9 C21 C16 120.8(6) . .
C8 C24 C22 119.5(5) . 2_766
C26 C27 N4 110.5(5) . .
N7 C28 C9 113.4(5) . 1_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N4 2.230(4) .
Mn1 N3 2.233(4) .
Mn1 N6 2.255(5) .
Mn1 B18 2.516(8) .
Mn1 B26 2.556(8) .
N2 C18 1.336(7) .
N2 C11 1.361(6) .
N2 C15 1.460(7) .
N3 C18 1.313(7) .
N3 C17 1.365(7) .
N4 C25 1.311(7) .
N4 C27 1.367(7) .
N7 C25 1.361(7) .
N7 C26 1.366(7) .
N7 C28 1.449(7) .
N5 C14 1.353(7) .
N5 C10 1.375(7) .
N5 C23 1.473(7) .
C7 C10 1.359(8) .
C7 N6 1.375(7) .
C8 C22 1.369(7) .
C8 C24 1.384(7) .
C9 C19 1.384(7) .
C9 C21 1.385(7) .
C9 C28 1.522(8) 1_454
C11 C17 1.350(7) .
N6 C14 1.308(7) .
C13 C20 1.380(7) .
C13 C19 1.392(8) .
C15 C20 1.517(8) .
C16 C21 1.388(8) .
C16 C20 1.392(7) .
C26 C27 1.345(8) .
C22 C24 1.393(7) 2_766
C22 C23 1.523(8) .
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_4
N6 C7 C10 N5 1.1(7) . .
C14 N5 C10 C7 -0.7(7) . .
C23 N5 C10 C7 176.7(5) . .
C18 N2 C11 C17 0.2(6) . .
C15 N2 C11 C17 176.0(5) . .
C10 C7 N6 C14 -1.1(6) . .
C10 C7 N6 Mn1 164.6(4) . .
C7 N6 C14 N5 0.6(6) . .
Mn1 N6 C14 N5 -166.2(3) . .
C10 N5 C14 N6 0.0(7) . .
C23 N5 C14 N6 -177.5(5) . .
C18 N2 C15 C20 95.1(7) . .
C11 N2 C15 C20 -80.1(7) . .
C27 N4 C25 N7 0.4(6) . .
Mn1 N4 C25 N7 161.9(3) . .
C26 N7 C25 N4 0.5(6) . .
C28 N7 C25 N4 177.6(5) . .
C25 N7 C26 C27 -1.2(6) . .
C28 N7 C26 C27 -178.2(6) . .
N2 C11 C17 N3 -0.3(6) . .
C18 N3 C17 C11 0.2(7) . .
Mn1 N3 C17 C11 179.7(4) . .
C21 C9 C19 C13 -3.1(8) . .
C28 C9 C19 C13 -179.3(6) 1_454 .
C20 C13 C19 C9 2.3(9) . .
C19 C13 C20 C16 -0.5(8) . .
C19 C13 C20 C15 178.9(5) . .
C21 C16 C20 C13 -0.5(8) . .
C21 C16 C20 C15 -180.0(6) . .
N2 C15 C20 C13 119.8(6) . .
N2 C15 C20 C16 -60.8(7) . .
C24 C8 C22 C24 -0.9(9) . 2_766
C24 C8 C22 C23 177.8(5) . .
C14 N5 C23 C22 77.4(7) . .
C10 N5 C23 C22 -99.6(7) . .
C8 C22 C23 N5 57.7(8) . .
C24 C22 C23 N5 -123.6(6) 2_766 .
C17 N3 C18 N2 -0.1(7) . .
Mn1 N3 C18 N2 -179.6(3) . .
C11 N2 C18 N3 -0.1(6) . .
C15 N2 C18 N3 -176.0(5) . .
C19 C9 C21 C16 2.1(8) . .
C28 C9 C21 C16 178.4(6) 1_454 .
C20 C16 C21 C9 -0.3(9) . .
C22 C8 C24 C22 1.0(9) . 2_766
N7 C26 C27 N4 1.5(7) . .
C25 N4 C27 C26 -1.2(7) . .
Mn1 N4 C27 C26 -161.2(4) . .
C25 N7 C28 C9 122.8(6) . 1_656
C26 N7 C28 C9 -60.8(8) . 1_656
