#------------------------------------------------------------------------------
#$Date: 2022-02-03 22:02:17 +0200 (Thu, 03 Feb 2022) $
#$Revision: 272445 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/92/4519275.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_4519275
loop_
_publ_author_name
'Wang, Yefei'
'Zhao, Liang'
'Ji, Guanfeng'
'He, Cheng'
'Liu, Songtao'
'Duan, Chunying'
_publ_section_title
;
 Vanadium(VIV)-Porphyrin-Based Metal-Organic Frameworks for
 Synergistic Bimetallic Activation of Inert C(sp³)-H Bonds.
;
_journal_issue                   2
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              2794
_journal_page_last               2804
_journal_paper_doi               10.1021/acsami.1c20420
_journal_volume                  14
_journal_year                    2022
_chemical_formula_sum            'C48 H24 Mn2 N4 O11.67 V'
_chemical_formula_weight         1004.20
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   32.603(12)
_cell_length_b                   32.603(12)
_cell_length_c                   16.679(8)
_cell_measurement_reflns_used    6540
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      2.44
_cell_volume                     15354(11)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2454
_diffrn_reflns_av_unetI/netI     0.1327
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            88718
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.266
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    0.326
_exptl_crystal_description       block
_exptl_crystal_F_000             1519
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.433
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.1362
_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)+(0.0500P)²+0.2000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2987
_refine_ls_wR_factor_ref         0.3123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1567
_reflns_number_total             5098
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am1c20420_si_002.cif
_cod_data_source_block           Mn-TCPP(V)
_cod_original_cell_volume        15354(14)
_cod_database_code               4519275
_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   0.965
_shelx_estimated_absorpt_t_max   0.982
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z'
'-y, x-y, z'
'-x, -y, z'
'-x+y, -x, z'
'y, -x+y, z'
'x-y, -y, -z'
'x, x-y, -z'
'y, x, -z'
'-x+y, y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x, -y, -z'
'-x+y, -x, -z'
'y, -x+y, -z'
'x, y, -z'
'x-y, x, -z'
'-y, x-y, -z'
'-x+y, y, z'
'-x, -x+y, z'
'-y, -x, z'
'x-y, -y, z'
'x, x-y, z'
'y, x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.40768(7) 0.70384(4) 0.5000 0.1596(9) Uani 1 4 d S TU P . .
C10 C 0.3838(3) 0.7675(6) 0.6125(7) 0.197(6) Uani 1 2 d S TU P . .
V1 V 0.5000 1.0000 1.0000 0.2388(17) Uani 1 8 d S TU P . .
C7 C 0.4633(2) 0.8618(3) 0.7665(5) 0.226(4) Uani 1 1 d D . . . .
H7 H 0.4951 0.8742 0.7842 0.272 Uiso 1 1 calc R U . . .
O3 O 0.3333 0.6667 0.5000 0.144(3) Uani 1 12 d S TU P . .
C8 C 0.4448(3) 0.8230(3) 0.7039(5) 0.210(3) Uani 1 1 d D U . . .
H8 H 0.4650 0.8116 0.6860 0.252 Uiso 1 1 calc R U . . .
O1 O 0.4103(2) 0.7517(2) 0.5899(3) 0.190(2) Uani 1 1 d . U . . .
C6 C 0.4396(2) 0.8792(4) 0.7972(6) 0.175(4) Uani 1 2 d DS T P . .
O2 O 0.5594(4) 1.0000 1.0000 0.114(4) Uani 0.5 4 d S TU P . .
N1 N 0.4649(2) 0.9298(4) 1.0000 0.2388(17) Uani 1 4 d S TU P . .
O4 O 0.4848(4) 0.7424(2) 0.5000 0.292(6) Uani 1 4 d S TU P . .
N2 N 0.5000 1.0000 0.8769(6) 0.2388(17) Uani 1 4 d S TU P . .
C9 C 0.4021(2) 0.8043(4) 0.6734(6) 0.157(3) Uani 1 2 d DS TU P . .
C5 C 0.48898(12) 0.9780(2) 0.7457(4) 0.195(4) Uani 1 2 d S T P . .
H5 H 0.4792 0.9584 0.6994 0.233 Uiso 1 2 calc R U P . .
C3 C 0.45827(19) 0.9165(4) 0.8549(5) 0.204(5) Uani 1 2 d S TU P . .
C4 C 0.4806(2) 0.9612(4) 0.8285(5) 0.176(3) Uani 1 2 d S TU P . .
C2 C 0.45145(19) 0.9029(4) 0.9346(5) 0.224(3) Uani 1 2 d S TU P . .
C1 C 0.4256(2) 0.8512(4) 0.9620(4) 0.270(6) Uani 1 2 d S TU P . .
H1 H 0.4120 0.8241 0.9282 0.324 Uiso 1 2 calc R U 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
O3 Mn1 O1 92.01(18) . 16_556 ?
O3 Mn1 O1 92.01(18) . 8_566 ?
O1 Mn1 O1 90.6(3) 16_556 8_566 ?
O3 Mn1 O1 92.01(18) . 23_565 ?
O1 Mn1 O1 176.0(4) 16_556 23_565 ?
O1 Mn1 O1 89.3(3) 8_566 23_565 ?
O3 Mn1 O1 92.01(18) . . ?
O1 Mn1 O1 89.3(3) 16_556 . ?
O1 Mn1 O1 176.0(4) 8_566 . ?
O1 Mn1 O1 90.6(3) 23_565 . ?
O3 Mn1 O4 180.0 . . ?
O1 Mn1 O4 87.99(18) 16_556 . ?
O1 Mn1 O4 87.99(18) 8_566 . ?
O1 Mn1 O4 87.99(18) 23_565 . ?
O1 Mn1 O4 87.99(18) . . ?
O1 C10 O1 125.1(15) . 19 ?
O1 C10 C9 117.4(7) . . ?
O1 C10 C9 117.4(7) 19 . ?
O2 V1 O2 180.0 13_677 . ?
O2 V1 N1 90.000(3) 13_677 . ?
O2 V1 N1 90.000(2) . . ?
O2 V1 N1 90.001(2) 13_677 13_677 ?
O2 V1 N1 89.999(3) . 13_677 ?
N1 V1 N1 180.0 . 13_677 ?
O2 V1 N2 90.000(3) 13_677 13_677 ?
O2 V1 N2 90.000(3) . 13_677 ?
N1 V1 N2 90.000(3) . 13_677 ?
N1 V1 N2 90.000(3) 13_677 13_677 ?
O2 V1 N2 90.000(3) 13_677 . ?
O2 V1 N2 90.000(3) . . ?
N1 V1 N2 90.000(3) . . ?
N1 V1 N2 90.000(3) 13_677 . ?
N2 V1 N2 180.0 13_677 . ?
C6 C7 C8 124.9(7) . . ?
C6 C7 H7 117.5 . . ?
C8 C7 H7 117.5 . . ?
Mn1 O3 Mn1 120.0 3_665 14_566 ?
Mn1 O3 Mn1 120.000(1) 3_665 . ?
Mn1 O3 Mn1 120.0 14_566 . ?
C9 C8 C7 122.8(9) . . ?
C9 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
C10 O1 Mn1 136.1(9) . . ?
C7 C6 C7 112.3(10) . 19 ?
C7 C6 C3 123.8(5) . . ?
C7 C6 C3 123.8(5) 19 . ?
C2 N1 C2 110.3(12) 16_557 . ?
C2 N1 V1 124.8(6) 16_557 . ?
C2 N1 V1 124.8(6) . . ?
C4 N2 C4 107.1(12) 4_675 . ?
C4 N2 V1 126.4(6) 4_675 . ?
C4 N2 V1 126.4(6) . . ?
C8 C9 C8 112.1(12) 19 . ?
C8 C9 C10 124.0(6) 19 . ?
C8 C9 C10 124.0(6) . . ?
C5 C5 C4 108.9(5) 4_675 . ?
C5 C5 H5 125.5 4_675 . ?
C4 C5 H5 125.5 . . ?
C4 C3 C2 125.4(9) . . ?
C4 C3 C6 118.4(9) . . ?
C2 C3 C6 116.2(10) . . ?
C3 C4 N2 124.3(8) . . ?
C3 C4 C5 128.2(9) . . ?
N2 C4 C5 107.5(10) . . ?
N1 C2 C3 129.0(10) . . ?
N1 C2 C1 107.5(8) . . ?
C3 C2 C1 123.5(8) . . ?
C1 C1 C2 107.4(4) 16_557 . ?
C1 C1 H1 126.3 16_557 . ?
C2 C1 H1 126.3 . . ?
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 O3 2.099(2) . ?
Mn1 O1 2.135(6) 16_556 ?
Mn1 O1 2.135(6) 8_566 ?
Mn1 O1 2.135(6) 23_565 ?
Mn1 O1 2.135(6) . ?
Mn1 O4 2.179(12) . ?
C10 O1 1.267(7) . ?
C10 O1 1.267(7) 19 ?
C10 C9 1.453(17) . ?
V1 O2 1.938(14) 13_677 ?
V1 O2 1.938(14) . ?
V1 N1 1.982(12) . ?
V1 N1 1.982(12) 13_677 ?
V1 N2 2.053(10) 13_677 ?
V1 N2 2.053(10) . ?
C7 C6 1.273(6) . ?
C7 C8 1.515(11) . ?
C7 H7 0.9500 . ?
O3 Mn1 2.099(2) 3_665 ?
O3 Mn1 2.099(2) 14_566 ?
C8 C9 1.311(6) . ?
C8 H8 0.9500 . ?
C6 C7 1.273(6) 19 ?
C6 C3 1.427(12) . ?
N1 C2 1.329(10) 16_557 ?
N1 C2 1.329(10) . ?
N2 C4 1.361(10) 4_675 ?
N2 C4 1.361(10) . ?
C9 C8 1.311(6) 19 ?
C5 C5 1.245(14) 4_675 ?
C5 C4 1.459(10) . ?
C5 H5 0.9500 . ?
C3 C4 1.336(11) . ?
C3 C2 1.384(11) . ?
C2 C1 1.530(13) . ?
C1 C1 1.269(14) 16_557 ?
C1 H1 0.9500 . ?
