#------------------------------------------------------------------------------
#$Date: 2019-01-11 01:25:39 +0200 (Fri, 11 Jan 2019) $
#$Revision: 212906 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/27/7122796.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_7122796
loop_
_publ_author_name
'Kumar, Amit'
'Sil, Debangsu'
'Usman, Mohammad'
'Rath, Sankar Prasad'
_publ_section_title
;
 Dimanganese(III) porphyrin dication diradical and its transformation to a
 μ-hydroxo porphyrin-oxophlorin heterodimer
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09366K
_journal_year                    2019
_chemical_formula_sum            'C74 H88 Cl2 Mn2 N8'
_chemical_formula_weight         1270.30
_chemical_name_systematic
;
 ?
;
_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   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-10-24 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                97.286(4)
_cell_angle_beta                 101.380(4)
_cell_angle_gamma                106.260(4)
_cell_formula_units_Z            1
_cell_length_a                   12.2256(19)
_cell_length_b                   13.0137(19)
_cell_length_c                   13.2500(19)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.5
_cell_volume                     1946.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24030
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.506
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0650
_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)+(0.0801P)²+3.8204P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5078
_reflns_number_total             7219
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc09366k2.cif
_cod_data_source_block           shelx
_cod_database_code               7122796
_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   0.910
_shelx_estimated_absorpt_t_max   0.950
_shelxl_version_number           2014-3
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 0.90060(5) 0.01894(5) 0.15701(5) 0.01642(16) Uani 1 1 d . .
Cl1 Cl 0.80662(11) 0.13275(9) 0.24722(9) 0.0345(3) Uani 1 1 d . .
N1 N 0.7601(3) -0.1121(3) 0.1314(3) 0.0175(7) Uani 1 1 d . .
N2 N 0.9797(3) -0.0331(3) 0.2778(3) 0.0195(7) Uani 1 1 d . .
N3 N 1.0570(3) 0.1247(3) 0.1618(3) 0.0186(7) Uani 1 1 d . .
N4 N 0.8370(3) 0.0460(3) 0.0162(2) 0.0162(7) Uani 1 1 d . .
C1 C 0.6503(3) -0.1222(3) 0.0713(3) 0.0172(8) Uani 1 1 d . .
C2 C 0.5644(3) -0.2169(3) 0.0882(3) 0.0213(9) Uani 1 1 d . .
C3 C 0.6231(4) -0.2635(3) 0.1567(3) 0.0216(9) Uani 1 1 d . .
C4 C 0.7440(4) -0.1949(3) 0.1878(3) 0.0198(9) Uani 1 1 d . .
C5 C 0.8287(4) -0.2034(3) 0.2694(3) 0.0213(9) Uani 1 1 d . .
H5 H 0.8113 -0.2690 0.2961 0.026 Uiso 1 1 calc R U
C6 C 0.9351(4) -0.1266(3) 0.3155(3) 0.0202(9) Uani 1 1 d . .
C7 C 1.0126(4) -0.1263(3) 0.4122(3) 0.0228(9) Uani 1 1 d . .
C8 C 1.1029(4) -0.0306(3) 0.4355(3) 0.0234(9) Uani 1 1 d . .
C9 C 1.0840(4) 0.0255(3) 0.3497(3) 0.0219(9) Uani 1 1 d . .
C10 C 1.1603(4) 0.1195(3) 0.3369(3) 0.0227(9) Uani 1 1 d . .
H10 H 1.2254 0.1576 0.3944 0.027 Uiso 1 1 calc R U
C11 C 1.1506(4) 0.1638(3) 0.2470(3) 0.0206(9) Uani 1 1 d . .
C12 C 1.2409(4) 0.2506(3) 0.2257(3) 0.0231(9) Uani 1 1 d . .
C13 C 1.2030(3) 0.2610(3) 0.1253(3) 0.0210(9) Uani 1 1 d . .
C14 C 1.0865(3) 0.1827(3) 0.0863(3) 0.0186(9) Uani 1 1 d . .
C15 C 1.0123(3) 0.1743(3) -0.0095(3) 0.0185(9) Uani 1 1 d . .
H15 H 1.0449 0.2131 -0.0582 0.022 Uiso 1 1 calc R U
C16 C 0.8943(3) 0.1141(3) -0.0407(3) 0.0175(8) Uani 1 1 d . .
C17 C 0.8121(4) 0.1226(3) -0.1306(3) 0.0190(9) Uani 1 1 d . .
C18 C 0.7033(4) 0.0642(3) -0.1253(3) 0.0197(9) Uani 1 1 d . .
C19 C 0.7190(3) 0.0158(3) -0.0321(3) 0.0169(8) Uani 1 1 d . .
C20 C 0.6303(3) -0.0536(3) 0.0024(3) 0.0183(9) Uani 1 1 d . .
C21 C 0.4361(4) -0.2642(3) 0.0308(3) 0.0252(10) Uani 1 1 d . .
H21A H 0.4010 -0.2044 0.0272 0.030 Uiso 1 1 calc R U
H21B H 0.3944 -0.3145 0.0710 0.030 Uiso 1 1 calc R U
C22 C 0.4181(4) -0.3256(4) -0.0798(4) 0.0338(11) Uani 1 1 d . .
H22A H 0.3341 -0.3513 -0.1148 0.051 Uiso 1 1 calc R U
H22B H 0.4474 -0.3883 -0.0765 0.051 Uiso 1 1 calc R U
H22C H 0.4611 -0.2769 -0.1194 0.051 Uiso 1 1 calc R U
C23 C 0.5752(4) -0.3630(3) 0.1995(4) 0.0287(10) Uani 1 1 d . .
H23A H 0.6361 -0.3995 0.2139 0.034 Uiso 1 1 calc R U
H23B H 0.5070 -0.4145 0.1460 0.034 Uiso 1 1 calc R U
C24 C 0.5366(5) -0.3367(4) 0.3011(4) 0.0450(14) Uani 1 1 d . .
H24A H 0.5063 -0.4043 0.3261 0.067 Uiso 1 1 calc R U
H24B H 0.4748 -0.3023 0.2869 0.067 Uiso 1 1 calc R U
H24C H 0.6041 -0.2868 0.3548 0.067 Uiso 1 1 calc R U
C25 C 0.9928(4) -0.2165(4) 0.4737(3) 0.0261(10) Uani 1 1 d . .
H25A H 0.9093 -0.2404 0.4765 0.031 Uiso 1 1 calc R U
H25B H 1.0414 -0.1883 0.5465 0.031 Uiso 1 1 calc R U
C26 C 1.0236(5) -0.3139(4) 0.4259(4) 0.0413(13) Uani 1 1 d . .
H26A H 1.0121 -0.3694 0.4697 0.062 Uiso 1 1 calc R U
H26B H 1.1059 -0.2905 0.4220 0.062 Uiso 1 1 calc R U
H26C H 0.9727 -0.3446 0.3552 0.062 Uiso 1 1 calc R U
C27 C 1.2069(4) 0.0114(4) 0.5275(3) 0.0287(10) Uani 1 1 d . .
H27A H 1.1849 -0.0184 0.5884 0.034 Uiso 1 1 calc R U
H27B H 1.2277 0.0917 0.5456 0.034 Uiso 1 1 calc R U
C28 C 1.3151(4) -0.0177(4) 0.5094(4) 0.0403(12) Uani 1 1 d . .
H28A H 1.3817 0.0185 0.5700 0.060 Uiso 1 1 calc R U
H28B H 1.3344 0.0067 0.4462 0.060 Uiso 1 1 calc R U
H28C H 1.2987 -0.0969 0.5003 0.060 Uiso 1 1 calc R U
C29 C 1.3540(4) 0.3168(4) 0.3051(4) 0.0295(10) Uani 1 1 d . .
H29A H 1.3886 0.2664 0.3402 0.035 Uiso 1 1 calc R U
H29B H 1.4103 0.3556 0.2676 0.035 Uiso 1 1 calc R U
C30 C 1.3384(4) 0.3987(4) 0.3872(4) 0.0403(13) Uani 1 1 d . .
H30A H 1.4146 0.4384 0.4360 0.060 Uiso 1 1 calc R U
H30B H 1.2841 0.3609 0.4258 0.060 Uiso 1 1 calc R U
H30C H 1.3063 0.4503 0.3533 0.060 Uiso 1 1 calc R U
C31 C 1.2622(4) 0.3407(3) 0.0667(4) 0.0264(10) Uani 1 1 d . .
H31A H 1.2394 0.3070 -0.0088 0.032 Uiso 1 1 calc R U
H31B H 1.3483 0.3574 0.0914 0.032 Uiso 1 1 calc R U
C32 C 1.2319(5) 0.4470(4) 0.0798(4) 0.0387(12) Uani 1 1 d . .
H32A H 1.2744 0.4968 0.0407 0.058 Uiso 1 1 calc R U
H32B H 1.2546 0.4810 0.1543 0.058 Uiso 1 1 calc R U
H32C H 1.1471 0.4315 0.0527 0.058 Uiso 1 1 calc R U
C33 C 0.8428(4) 0.1912(3) -0.2101(3) 0.0218(9) Uani 1 1 d . .
H33A H 0.7957 0.1509 -0.2810 0.026 Uiso 1 1 calc R U
H33B H 0.9269 0.2047 -0.2093 0.026 Uiso 1 1 calc R U
C34 C 0.8196(5) 0.3003(4) -0.1878(4) 0.0353(12) Uani 1 1 d . .
H34A H 0.8417 0.3433 -0.2403 0.053 Uiso 1 1 calc R U
H34B H 0.8662 0.3403 -0.1177 0.053 Uiso 1 1 calc R U
H34C H 0.7359 0.2871 -0.1910 0.053 Uiso 1 1 calc R U
C35 C 0.5921(4) 0.0417(3) -0.2079(3) 0.0229(9) Uani 1 1 d . .
H35A H 0.6050 0.0934 -0.2563 0.027 Uiso 1 1 calc R U
H35B H 0.5299 0.0533 -0.1743 0.027 Uiso 1 1 calc R U
C36 C 0.5518(4) -0.0746(4) -0.2698(4) 0.0331(11) Uani 1 1 d . .
H36A H 0.4786 -0.0872 -0.3227 0.050 Uiso 1 1 calc R U
H36B H 0.5384 -0.1259 -0.2221 0.050 Uiso 1 1 calc R U
H36C H 0.6124 -0.0857 -0.3047 0.050 Uiso 1 1 calc R U
C37 C 0.5106(3) -0.0415(3) -0.0264(3) 0.0213(9) Uani 1 1 d . .
H37A H 0.4508 -0.0923 -0.0816 0.026 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'
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'
Cl Cl 0.1484 0.1585 '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
N4 Mn1 N1 88.63(13) .
N4 Mn1 N2 165.73(13) .
N1 Mn1 N2 89.85(13) .
N4 Mn1 N3 89.60(13) .
N1 Mn1 N3 165.44(13) .
N2 Mn1 N3 88.31(13) .
N4 Mn1 Cl1 93.80(10) .
N1 Mn1 Cl1 91.69(10) .
N2 Mn1 Cl1 100.42(10) .
N3 Mn1 Cl1 102.84(10) .
C4 N1 C1 106.2(3) .
C4 N1 Mn1 127.4(3) .
C1 N1 Mn1 124.6(3) .
C9 N2 C6 105.8(3) .
C9 N2 Mn1 126.0(3) .
C6 N2 Mn1 127.7(3) .
C11 N3 C14 106.3(3) .
C11 N3 Mn1 126.0(3) .
C14 N3 Mn1 127.3(3) .
C16 N4 C19 106.3(3) .
C16 N4 Mn1 128.2(3) .
C19 N4 Mn1 124.2(3) .
N1 C1 C20 123.5(4) .
N1 C1 C2 109.4(3) .
C20 C1 C2 127.0(4) .
C3 C2 C1 107.2(3) .
C3 C2 C21 125.3(4) .
C1 C2 C21 127.1(4) .
C2 C3 C4 107.0(3) .
C2 C3 C23 128.4(4) .
C4 C3 C23 124.5(4) .
N1 C4 C5 124.5(4) .
N1 C4 C3 110.0(3) .
C5 C4 C3 125.2(4) .
C6 C5 C4 126.3(4) .
C5 C6 N2 123.9(4) .
C5 C6 C7 125.8(4) .
N2 C6 C7 110.2(4) .
C8 C7 C6 107.1(4) .
C8 C7 C25 128.4(4) .
C6 C7 C25 124.5(4) .
C7 C8 C9 106.8(4) .
C7 C8 C27 129.2(4) .
C9 C8 C27 123.9(4) .
C10 C9 N2 124.2(4) .
C10 C9 C8 125.7(4) .
N2 C9 C8 110.0(4) .
C9 C10 C11 125.4(4) .
N3 C11 C10 124.3(4) .
N3 C11 C12 110.0(3) .
C10 C11 C12 125.4(4) .
C13 C12 C11 107.3(4) .
C13 C12 C29 128.5(4) .
C11 C12 C29 124.3(4) .
C12 C13 C14 106.2(4) .
C12 C13 C31 128.4(4) .
C14 C13 C31 125.3(4) .
N3 C14 C15 124.9(4) .
N3 C14 C13 110.2(3) .
C15 C14 C13 124.7(4) .
C14 C15 C16 125.5(4) .
N4 C16 C15 124.2(4) .
N4 C16 C17 110.2(3) .
C15 C16 C17 125.2(4) .
C18 C17 C16 107.4(3) .
C18 C17 C33 127.2(4) .
C16 C17 C33 125.3(4) .
C17 C18 C19 106.5(4) .
C17 C18 C35 125.7(4) .
C19 C18 C35 127.2(4) .
N4 C19 C20 124.3(3) .
N4 C19 C18 109.4(3) .
C20 C19 C18 126.3(4) .
C1 C20 C19 123.7(4) .
C1 C20 C37 118.9(4) .
C19 C20 C37 116.9(3) .
C2 C21 C22 112.6(4) .
C3 C23 C24 112.6(4) .
C7 C25 C26 112.2(4) .
C8 C27 C28 114.1(4) .
C30 C29 C12 113.7(4) .
C13 C31 C32 113.1(4) .
C17 C33 C34 111.6(3) .
C18 C35 C36 111.4(3) .
C37 C37 C20 118.9(5) 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N4 1.988(3) .
Mn1 N1 1.990(3) .
Mn1 N2 1.996(3) .
Mn1 N3 2.003(3) .
Mn1 Cl1 2.4471(13) .
N1 C4 1.379(5) .
N1 C1 1.379(5) .
N2 C9 1.381(5) .
N2 C6 1.385(5) .
N3 C11 1.364(5) .
N3 C14 1.372(5) .
N4 C16 1.370(5) .
N4 C19 1.378(5) .
C1 C20 1.390(5) .
C1 C2 1.452(5) .
C2 C3 1.354(6) .
C2 C21 1.513(6) .
C3 C4 1.441(6) .
C3 C23 1.495(6) .
C4 C5 1.380(6) .
C5 C6 1.367(6) .
C6 C7 1.434(6) .
C7 C8 1.366(6) .
C7 C25 1.504(6) .
C8 C9 1.442(6) .
C8 C27 1.494(6) .
C9 C10 1.368(6) .
C10 C11 1.387(6) .
C11 C12 1.441(6) .
C12 C13 1.358(6) .
C12 C29 1.513(6) .
C13 C14 1.448(6) .
C13 C31 1.486(6) .
C14 C15 1.378(6) .
C15 C16 1.384(6) .
C16 C17 1.435(6) .
C17 C18 1.356(6) .
C17 C33 1.502(5) .
C18 C19 1.459(5) .
C18 C35 1.496(6) .
C19 C20 1.398(6) .
C20 C37 1.495(5) .
C21 C22 1.521(6) .
C23 C24 1.541(7) .
C25 C26 1.519(7) .
C27 C28 1.527(7) .
C29 C30 1.503(7) .
C31 C32 1.528(6) .
C33 C34 1.529(6) .
C35 C36 1.521(6) .
C37 C37 1.327(8) 2_655
