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#$Date: 2024-03-04 22:25:12 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290212 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/49/7714998.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_7714998
loop_
_publ_author_name
'Imamura, Yuki'
'Yoshino, Haruka'
'Le Ouay, Benjamin'
'Ohtani, Ryo'
'Ohba, Masaaki'
_publ_section_title
;
 A novel style of 2D Hofmann-type coordination polymer incorporated
 trigonal prismatic coordination geometry with bidentate co-ligands.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3970
_journal_page_last               3974
_journal_paper_doi               10.1039/d3dt03914e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '0.5(C32 H24 Mn4 N14)'
_chemical_formula_sum            'C16 H12 Mn2 N7'
_chemical_formula_weight         412.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-22 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.990
_cell_length_b                   7.058
_cell_length_c                   16.715
_cell_measurement_reflns_used    3848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.41
_cell_volume                     1650.463
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.969
_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_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17116
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.362
_diffrn_reflns_theta_min         1.898
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1263 before and 0.0649 after correction. The Ratio of minimum to maximum transmission is 0.8338. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'pinkish orange'
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.0973
_exptl_crystal_size_min          0.0875
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+0.8429P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1997
_reflns_number_total             2367
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03914e2.cif
_cod_data_source_block           MnMn_dmbpy
_cod_depositor_comments
'Adding full bibliography for 7714998--7714999.cif.'
_cod_original_cell_volume        1650.4
_cod_database_code               7714998
_shelx_shelxl_version_number     2018/3
_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_max   0.877
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C13(H13A,H13B,H13C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
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 0.39793(2) 0.250000 0.68110(2) 0.00942(11) Uani 1 2 d S T P . .
Mn2 Mn 0.62139(2) 0.750000 0.81595(2) 0.01130(11) Uani 1 2 d S T P . .
N4 N 0.34484(14) 0.250000 0.55431(13) 0.0148(4) Uani 1 2 d S T P . .
N5 N 0.52457(15) 0.250000 0.59577(12) 0.0147(4) Uani 1 2 d S T P . .
N1 N 0.48078(10) 0.4579(2) 0.74744(9) 0.0179(3) Uani 1 1 d . . . . .
N3 N 0.60311(15) 0.750000 0.90314(14) 0.0199(5) Uani 1 2 d S T P . .
N2 N 0.78302(11) 1.0423(2) 0.80083(10) 0.0180(3) Uani 1 1 d . . . . .
C1 C 0.53232(12) 0.5631(2) 0.77505(11) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.72229(12) 0.9366(3) 0.80502(11) 0.0158(3) Uani 1 1 d . . . . .
C3 C 0.25241(17) 0.250000 0.53704(16) 0.0173(5) Uani 1 2 d S T P . .
H3 H 0.208230 0.250000 0.580201 0.021 Uiso 1 2 calc RS T P . .
C4 C 0.21682(19) 0.250000 0.46101(17) 0.0204(5) Uani 1 2 d S T P . .
C5 C 0.1121(2) 0.250000 0.4467(2) 0.0296(7) Uani 1 2 d S T P . .
H5A H 0.079880 0.182866 0.490364 0.044 Uiso 0.5 1 calc GR . . A -1
H5B H 0.098332 0.186230 0.395884 0.044 Uiso 0.5 1 calc GR . . A -1
H5C H 0.088869 0.380903 0.444338 0.044 Uiso 0.5 1 calc GR . . A -1
C6 C 0.2821(2) 0.250000 0.39997(17) 0.0234(6) Uani 1 2 d S T P . .
H6 H 0.260994 0.250000 0.345956 0.028 Uiso 1 2 calc RS T P . .
C7 C 0.3772(2) 0.250000 0.41673(16) 0.0221(6) Uani 1 2 d S T P . .
H7 H 0.422657 0.250000 0.374518 0.027 Uiso 1 2 calc RS T P . .
C8 C 0.40692(17) 0.250000 0.49418(15) 0.0141(5) Uani 1 2 d S T P . .
C9 C 0.50765(17) 0.250000 0.51780(15) 0.0139(5) Uani 1 2 d S T P . .
C10 C 0.58088(19) 0.250000 0.46350(16) 0.0205(5) Uani 1 2 d S T P . .
H10 H 0.567963 0.250000 0.407700 0.025 Uiso 1 2 calc RS T P . .
C11 C 0.67245(19) 0.250000 0.49082(16) 0.0208(5) Uani 1 2 d S T P . .
H11 H 0.723860 0.250000 0.453688 0.025 Uiso 1 2 calc RS T P . .
C12 C 0.69141(17) 0.250000 0.57099(15) 0.0171(5) Uani 1 2 d S T P . .
C13 C 0.78982(18) 0.250000 0.60370(17) 0.0230(6) Uani 1 2 d S T P . .
H13A H 0.835287 0.220953 0.560826 0.034 Uiso 0.5 1 calc GR . . B -1
H13B H 0.794946 0.153971 0.645837 0.034 Uiso 0.5 1 calc GR . . B -1
H13C H 0.804315 0.375076 0.626095 0.034 Uiso 0.5 1 calc GR . . B -1
C14 C 0.61348(17) 0.250000 0.62084(16) 0.0169(5) Uani 1 2 d S T P . .
H14 H 0.624553 0.250000 0.676911 0.020 Uiso 1 2 calc RS T P . .
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'
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'
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
N4 Mn1 N5 70.48(7) . . ?
N1 Mn1 N4 131.12(5) . . ?
N1 Mn1 N4 131.12(5) 7_565 . ?
N1 Mn1 N5 84.52(6) 7_565 . ?
N1 Mn1 N5 84.52(6) . . ?
N1 Mn1 N1 84.90(8) 7_565 . ?
N1 Mn1 N2 140.40(6) . 6_547 ?
N1 Mn1 N2 82.52(6) 7_565 6_547 ?
N1 Mn1 N2 140.40(6) 7_565 4_466 ?
N1 Mn1 N2 82.51(5) . 4_466 ?
N2 Mn1 N4 83.55(6) 4_466 . ?
N2 Mn1 N4 83.55(6) 6_547 . ?
N2 Mn1 N5 131.03(5) 6_547 . ?
N2 Mn1 N5 131.03(5) 4_466 . ?
N2 Mn1 N2 83.71(8) 6_547 4_466 ?
N3 Mn2 C1 103.66(8) . . ?
N3 Mn2 C1 103.66(8) . 7_575 ?
N3 Mn2 C2 102.62(8) . . ?
N3 Mn2 C2 102.62(8) . 7_575 ?
C1 Mn2 C1 85.74(10) . 7_575 ?
C2 Mn2 C1 88.43(7) . 7_575 ?
C2 Mn2 C1 153.72(8) . . ?
C2 Mn2 C1 88.43(7) 7_575 . ?
C2 Mn2 C1 153.72(8) 7_575 7_575 ?
C2 Mn2 C2 85.55(10) . 7_575 ?
C3 N4 Mn1 121.90(17) . . ?
C3 N4 C8 118.3(2) . . ?
C8 N4 Mn1 119.85(16) . . ?
C9 N5 Mn1 118.54(16) . . ?
C14 N5 Mn1 122.55(17) . . ?
C14 N5 C9 118.9(2) . . ?
C1 N1 Mn1 171.57(15) . . ?
C2 N2 Mn1 168.50(14) . 6_667 ?
N1 C1 Mn2 176.52(17) . . ?
N2 C2 Mn2 177.48(16) . . ?
N4 C3 C4 124.0(2) . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 C6 116.8(2) . . ?
C6 C4 C5 122.6(3) . . ?
C7 C6 C4 119.9(3) . . ?
C6 C7 C8 119.7(3) . . ?
N4 C8 C7 121.3(2) . . ?
N4 C8 C9 115.2(2) . . ?
C7 C8 C9 123.5(2) . . ?
N5 C9 C8 115.9(2) . . ?
N5 C9 C10 121.2(2) . . ?
C10 C9 C8 122.8(2) . . ?
C11 C10 C9 118.8(2) . . ?
C10 C11 C12 120.8(2) . . ?
C11 C12 C13 122.9(2) . . ?
C11 C12 C14 116.2(2) . . ?
C14 C12 C13 121.0(2) . . ?
N5 C14 C12 124.0(2) . . ?
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 N4 2.246(2) . ?
Mn1 N5 2.275(2) . ?
Mn1 N1 2.1740(15) . ?
Mn1 N1 2.1740(15) 7_565 ?
Mn1 N2 2.1963(15) 4_466 ?
Mn1 N2 2.1963(15) 6_547 ?
Mn2 N3 1.480(2) . ?
Mn2 C1 1.9392(18) . ?
Mn2 C1 1.9393(18) 7_575 ?
Mn2 C2 1.9391(18) 7_575 ?
Mn2 C2 1.9391(18) . ?
N4 C3 1.325(3) . ?
N4 C8 1.328(3) . ?
N5 C9 1.325(3) . ?
N5 C14 1.313(3) . ?
N1 C1 1.133(2) . ?
N2 C2 1.133(2) . ?
C3 C4 1.365(4) . ?
C4 C5 1.485(4) . ?
C4 C6 1.370(4) . ?
C6 C7 1.359(4) . ?
C7 C8 1.360(4) . ?
C8 C9 1.464(3) . ?
C9 C10 1.369(3) . ?
C10 C11 1.360(4) . ?
C11 C12 1.366(4) . ?
C12 C13 1.481(4) . ?
C12 C14 1.372(3) . ?
