#------------------------------------------------------------------------------
#$Date: 2024-05-05 03:43:42 +0300 (Sun, 05 May 2024) $
#$Revision: 291504 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/26/7132666.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_7132666
loop_
_publ_author_name
'Mine, Kosuke'
'Arae, Sachie'
'Murakawa, Hiroshi'
'Tsuchiizu, Masahisa'
'Hanasaki, Noriaki'
'Matsuda, Masaki'
_publ_section_title
;
 Diamond lattice in single-component molecular crystals comprising
 tetrabenzoporphyrin neutral radicals.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3019
_journal_page_last               3022
_journal_paper_doi               10.1039/d3cc05948k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C36 H20 Cl2 Mn N4'
_chemical_formula_sum            'C36 H20 Cl2 Mn N4'
_chemical_formula_weight         634.40
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-30 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7890(4)
_cell_length_b                   13.7890(4)
_cell_length_c                   14.4334(8)
_cell_measurement_reflns_used    3944
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8810
_cell_measurement_theta_min      2.0420
_cell_volume                     2744.32(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00  -1.00   0.50   80.00    --   12.19 -19.00  48.00  112
  2  ω     -5.00  37.00   0.50   80.00    --   12.19-110.00-131.00   84
  3  ω    -78.00 -39.00   0.50   80.00    --  -12.50 162.00-158.00   78
  4  ω     -1.00  25.00   0.50   80.00    --   12.19 -99.00 -30.00   52
  5  ω      2.00  75.00   0.50   80.00    --   12.19  37.00  30.00  146
  6  ω     14.00  40.00   0.50   80.00    --  -12.50  77.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089137000
_diffrn_orient_matrix_UB_12      -0.0503791000
_diffrn_orient_matrix_UB_13      0.0051097000
_diffrn_orient_matrix_UB_21      -0.0097629000
_diffrn_orient_matrix_UB_22      -0.0070267000
_diffrn_orient_matrix_UB_23      -0.0477758000
_diffrn_orient_matrix_UB_31      0.0497275000
_diffrn_orient_matrix_UB_32      0.0076286000
_diffrn_orient_matrix_UB_33      -0.0102625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6340
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.141
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0379
_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)+(0.0632P)²+1.3393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1181
_reflns_number_total             1589
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc05948k2.cif
_cod_data_source_block           MntbpCl2
_cod_depositor_comments
'Adding full bibliography for 7132664--7132666.cif.'
_cod_original_cell_volume        2744.3(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7132666
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H20Cl2Mn1N4
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.884
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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 0.500000 0.750000 0.625000 0.0372(2) Uani 1 4 d S T P . .
Cl1 Cl 0.500000 0.750000 0.80121(6) 0.0465(3) Uani 1 2 d S T P . .
N1 N 0.39980(13) 0.64277(12) 0.62866(12) 0.0380(4) Uani 1 1 d . . . . .
C1 C 0.30114(15) 0.65501(15) 0.63849(15) 0.0380(5) Uani 1 1 d . . . . .
C2 C 0.25512(15) 0.56095(15) 0.65121(15) 0.0373(5) Uani 1 1 d . . . . .
C3 C 0.15921(15) 0.53398(16) 0.66589(17) 0.0436(5) Uani 1 1 d . . . . .
H3 H 0.109803 0.579790 0.668804 0.052 Uiso 1 1 calc R U . . .
C4 C 0.14051(16) 0.43607(16) 0.67595(17) 0.0470(6) Uani 1 1 d . . . . .
H4 H 0.077039 0.415785 0.685936 0.056 Uiso 1 1 calc R U . . .
C5 C 0.21329(17) 0.36757(16) 0.67161(18) 0.0493(6) Uani 1 1 d . . . . .
H5 H 0.197944 0.302443 0.679690 0.059 Uiso 1 1 calc R U . . .
C6 C 0.30901(17) 0.39391(16) 0.65542(17) 0.0469(6) Uani 1 1 d . . . . .
H6 H 0.357924 0.347688 0.651228 0.056 Uiso 1 1 calc R U . . .
C7 C 0.32857(15) 0.49196(15) 0.64577(15) 0.0384(5) Uani 1 1 d . . . . .
C8 C 0.41825(15) 0.54479(15) 0.63073(15) 0.0382(5) Uani 1 1 d . . . . .
C9 C 0.50834(15) 0.50278(15) 0.61833(15) 0.0409(5) Uani 1 1 d . . . . .
H9 H 0.510401 0.435506 0.614231 0.049 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 '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
Cl1 Mn1 Cl1 180.0 15_566 . ?
N1 Mn1 Cl1 88.50(5) 6_564 . ?
N1 Mn1 Cl1 91.49(5) . 15_566 ?
N1 Mn1 Cl1 91.50(5) 6_564 15_566 ?
N1 Mn1 Cl1 91.50(5) 12_767 . ?
N1 Mn1 Cl1 91.50(5) 15_566 . ?
N1 Mn1 Cl1 88.50(5) 12_767 15_566 ?
N1 Mn1 Cl1 88.50(5) 15_566 15_566 ?
N1 Mn1 Cl1 88.51(5) . . ?
N1 Mn1 N1 90.038(3) . 15_566 ?
N1 Mn1 N1 90.039(3) 6_564 12_767 ?
N1 Mn1 N1 177.01(10) . 6_564 ?
N1 Mn1 N1 90.039(3) 6_564 15_566 ?
N1 Mn1 N1 177.01(10) 12_767 15_566 ?
N1 Mn1 N1 90.040(3) . 12_767 ?
C1 N1 Mn1 125.94(14) . . ?
C8 N1 Mn1 126.30(14) . . ?
C8 N1 C1 107.50(17) . . ?
N1 C1 C2 109.52(18) . . ?
C9 C1 N1 125.39(19) 15_566 . ?
C9 C1 C2 124.98(19) 15_566 . ?
C3 C2 C1 132.3(2) . . ?
C3 C2 C7 121.2(2) . . ?
C7 C2 C1 106.55(18) . . ?
C2 C3 H3 121.5 . . ?
C4 C3 C2 117.1(2) . . ?
C4 C3 H3 121.5 . . ?
C3 C4 H4 119.1 . . ?
C5 C4 C3 121.9(2) . . ?
C5 C4 H4 119.1 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.3(2) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 121.4 . . ?
C7 C6 C5 117.2(2) . . ?
C7 C6 H6 121.4 . . ?
C2 C7 C8 106.57(18) . . ?
C6 C7 C2 121.31(19) . . ?
C6 C7 C8 132.1(2) . . ?
N1 C8 C7 109.80(19) . . ?
N1 C8 C9 125.11(19) . . ?
C9 C8 C7 125.07(19) . . ?
C1 C9 C8 126.0(2) 12_767 . ?
C1 C9 H9 117.0 12_767 . ?
C8 C9 H9 117.0 . . ?
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 Cl1 2.5433(9) 15_566 ?
Mn1 Cl1 2.5433(9) . ?
Mn1 N1 2.0244(17) 12_767 ?
Mn1 N1 2.0244(17) 6_564 ?
Mn1 N1 2.0244(17) 15_566 ?
Mn1 N1 2.0244(17) . ?
N1 C1 1.378(3) . ?
N1 C8 1.375(3) . ?
C1 C2 1.455(3) . ?
C1 C9 1.372(3) 15_566 ?
C2 C3 1.390(3) . ?
C2 C7 1.392(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.389(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.386(3) . ?
C7 C8 1.452(3) . ?
C8 C9 1.382(3) . ?
C9 H9 0.9300 . ?
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
Mn1 N1 C1 C2 -171.94(14) . . . . ?
Mn1 N1 C1 C9 11.8(3) . . . 15_566 ?
Mn1 N1 C8 C7 172.24(14) . . . . ?
Mn1 N1 C8 C9 -9.1(3) . . . . ?
N1 C1 C2 C3 178.5(2) . . . . ?
N1 C1 C2 C7 -1.8(2) . . . . ?
N1 C8 C9 C1 7.1(4) . . . 12_767 ?
C1 N1 C8 C7 -2.1(2) . . . . ?
C1 N1 C8 C9 176.6(2) . . . . ?
C1 C2 C3 C4 -179.5(2) . . . . ?
C1 C2 C7 C6 179.8(2) . . . . ?
C1 C2 C7 C8 0.5(2) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C2 C7 C8 N1 1.0(2) . . . . ?
C2 C7 C8 C9 -177.8(2) . . . . ?
C3 C2 C7 C6 -0.5(4) . . . . ?
C3 C2 C7 C8 -179.7(2) . . . . ?
C3 C4 C5 C6 -1.0(4) . . . . ?
C4 C5 C6 C7 1.3(4) . . . . ?
C5 C6 C7 C2 -0.6(4) . . . . ?
C5 C6 C7 C8 178.4(2) . . . . ?
C6 C7 C8 N1 -178.2(2) . . . . ?
C6 C7 C8 C9 3.1(4) . . . . ?
C7 C2 C3 C4 0.8(4) . . . . ?
C7 C8 C9 C1 -174.4(2) . . . 12_767 ?
C8 N1 C1 C2 2.4(2) . . . . ?
C8 N1 C1 C9 -173.9(2) . . . 15_566 ?
C9 C1 C2 C3 -5.2(4) 15_566 . . . ?
C9 C1 C2 C7 174.5(2) 15_566 . . . ?
