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_7708754
_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         'C44 H28 Fe N4, C13 H30 P, C7 H8'
_chemical_formula_sum            'C64 H66 Fe N4 P'
_chemical_formula_weight         978.02
_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                 126.986(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9989(13)
_cell_length_b                   17.5588(12)
_cell_length_c                   27.870(3)
_cell_measurement_reflns_used    3783
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.8710
_cell_measurement_theta_min      1.9610
_cell_volume                     5081.2(13)
_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_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_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    -58.00  51.00   1.00  120.00    --   11.89   0.00-180.00  109
  2  \w   -102.00 -57.00   1.00  120.00    --  -12.20-178.00   0.00   45
  3  \w    -88.00 -62.00   1.00  120.00    --  -12.20 -37.00-150.00   26
  4  \w     16.00  48.00   1.00  120.00    --  -12.20-129.00 -19.00   32
  5  \w    -34.00  56.00   1.00  120.00    --   11.89 -19.00 -90.00   90
  6  \w     -5.00   0.00   1.00  120.00    --  -12.20 -99.00 150.00    5
;
_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      -0.0379763000
_diffrn_orient_matrix_UB_12      0.0118147000
_diffrn_orient_matrix_UB_13      -0.0304574000
_diffrn_orient_matrix_UB_21      -0.0229995000
_diffrn_orient_matrix_UB_22      -0.0377761000
_diffrn_orient_matrix_UB_23      -0.0093161000
_diffrn_orient_matrix_UB_31      -0.0519341000
_diffrn_orient_matrix_UB_32      0.0080828000
_diffrn_orient_matrix_UB_33      0.0011473000
_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  0.1108
_diffrn_reflns_av_unetI/netI     0.1899
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            36785
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.696
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.939
_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    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11350
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1925
_refine_ls_R_factor_gt           0.0803
_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/[\s^2^(Fo^2^)+(0.0506P)^2^+1.7214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5297
_reflns_number_total             11350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02573b2.cif
_cod_data_source_block           exp_1535_int1
_cod_original_cell_volume        5081.2(12)
_cod_database_code               7708754
_chemical_oxdiff_formula         'C256  H264  Fe4  N16  P4  '
_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 1.222
_oxdiff_exptl_absorpt_empirical_full_min 0.811
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21B-C210 \\sim C21A-C210
 with sigma of 0.02
 C23B-C22B \\sim C23A-C22A
 with sigma of 0.02
 C22B-C21B \\sim C22A-C21A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21B) = Uanis(C21A)
4. Others
 Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(H21G)=Sof(H21H)=1-FVAR(1)
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(H21E)=Sof(H21F)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C21B(H21C,H21D), C22A(H22A,H22B), C22B(H22C,H22D), C202(H20D,
 H20E), C203(H20F,H20G), C204(H20H,H20I), C206(H20M,H20N), C207(H20O,H20P),
 C208(H20Q,H20R), C210(H21E,H21F), C210(H21G,H21H)
5.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), C302(H302), C303(H303),
 C304(H304), C305(H305), C306(H306)
5.c Idealised Me refined as rotating group:
 C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F), C201(H20A,H20B,H20C), C205(H20J,
 H20K,H20L), C209(H20S,H20T,H20U), C307(H30A,H30B,H30C)
;
_shelx_res_checksum              53127