Macrocycle- and metal-centered reduction of metal tetraphenylporphyrins where the metal is copper(II), nickel(II) and iron(II).
Nazarov, Dmitry I.; Andronov, Mikhail G.; Kuzmin, Aleksey V.; Khasanov, Salavat S.; Yudanova, Evgeniya I.; Shestakov, Alexander F.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Konarev, Dmitri V.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 15620–15632; doi:10.1039/d1dt02573b

data_7708756
_publ_section_title
;
 Macrocycle- and metal-centered reduction of metal tetraphenylporphyrins
 where the metal is copper(II), nickel(II) and iron(II).
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15620
_journal_page_last               15632
_journal_paper_doi               10.1039/d1dt02573b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C62 H64 Cs N6 Ni O6, C7 H8'
_chemical_formula_sum            'C69 H72 Cs N6 Ni O6'
_chemical_formula_weight         1272.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-23
_audit_creation_method
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-07-23 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.12800(10)
_cell_length_b                   16.77500(10)
_cell_length_c                   27.6823(3)
_cell_measurement_reflns_used    23154
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.6610
_cell_measurement_theta_min      1.9870
_cell_volume                     5957.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -9.00  58.50   0.75   64.00    --   20.70  57.00 -30.00   90
  2  \w     55.00  82.00   0.75   64.00    --   20.70  37.00-120.00   36
  3  \w    -58.00  48.50   0.75   64.00    --   20.70 -57.00 150.00  142
  4  \w   -102.00 -69.00   0.75   64.00    --  -20.86 -57.00  60.00   44
  5  \w    -46.25 -12.50   0.75   64.00    --   20.70 -65.00  38.86   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0232796000
_diffrn_orient_matrix_UB_12      0.0362269000
_diffrn_orient_matrix_UB_13      0.0099820000
_diffrn_orient_matrix_UB_21      -0.0051312000
_diffrn_orient_matrix_UB_22      0.0155435000
_diffrn_orient_matrix_UB_23      -0.0242213000
_diffrn_orient_matrix_UB_31      -0.0498840000
_diffrn_orient_matrix_UB_32      0.0153143000
_diffrn_orient_matrix_UB_33      0.0009829000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            38728
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.710
_diffrn_reflns_theta_min         1.934
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.252
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         16662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+4.0514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14601
_reflns_number_total             16662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02573b2.cif
_cod_data_source_block           exp_1533_int1
_cod_database_code               7708756
_chemical_oxdiff_formula         C65H64N6O6Ni1Cs1
_shelx_shelxl_version_number     2018/3
_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 1.013
_oxdiff_exptl_absorpt_empirical_full_min 0.979
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_shelx_estimated_absorpt_t_min   0.668
_shelx_estimated_absorpt_t_max   0.789
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C207(H20M,H20N), C208(H20O,H20P), C209(H20Q,H20R),
 C210(H21A,H21B), C211(H21C,H21D), C212(H21E,H21F), C213(H21G,H21H), C214(H21I,
 H21J), C215(H21K,H21L), C216(H21M,H21N), C217(H21O,H21P), C218(H21Q,H21R)
2.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C108(H108), C109(H109), C113(H113), C114(H114),
 C118(H118), C119(H119), C122(H122), C123(H123), C124(H124), C125(H125),
 C126(H126), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 C134(H134), C135(H135), C136(H136), C137(H137), C138(H138), C140(H140),
 C141(H141), C142(H142), C143(H143), C144(H144), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              94833