A synchrotron study of [5,10,15,20-tetrakis(3-cyanophenyl)porphyrinato-κ^4^<i>N</i>^5^,<i>N</i>^10^,<i>N</i>^15^,<i>N</i>^20^]copper(II) nitrobenzene trisolvate at 80K
Seidel, Rüdiger W.; Goddard, Richard; Mayer-Gall, Thomas; Oppel, Iris M.; Acta Crystallographica Section C 72 (2016) 861–866; doi:10.1107/S2053229616015515

data_2020632
_publ_section_title
;
 A synchrotron study of
 [5,10,15,20-tetrakis(3-cyanophenyl)porphyrinato-\k^4^<i>N</i>^5^,<i>N</i>^10^,<i>N</i>^15^,<i>N</i>^20^]copper(II)
 nitrobenzene trisolvate at 80K
;
_journal_coeditor_code           YP3128
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              861
_journal_page_last               866
_journal_paper_doi               10.1107/S2053229616015515
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Cu (C48 H24 N8)], 3C6 H5 N O2'
_chemical_formula_moiety         'C48 H24 Cu N8, 3(C6 H5 N O2)'
_chemical_formula_sum            'C66 H39 Cu N11 O6'
_chemical_formula_weight         1145.62
_chemical_name_systematic
;
5,10,15,20-tetrakis(3-cyanophenyl)porphyrinatocopper(II) nitrobenzene trisolvate
;
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                104.37(3)
_cell_angle_beta                 94.85(10)
_cell_angle_gamma                96.85(8)
_cell_formula_units_Z            1
_cell_length_a                   8.234(4)
_cell_length_b                   11.872(9)
_cell_length_c                   14.212(7)
_cell_measurement_reflns_used    34070
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      23.723
_cell_measurement_theta_min      1.180
_cell_volume                     1326.8(14)
_computing_cell_refinement
;
XDS (Kabsch, 2010)
;
_computing_data_collection
;
P11 Crystallography Control (Meents <i>et al.</i>,  2013)
;
_computing_data_reduction
;
XDS (Kabsch, 2010)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
enCIFer (Allen <i>et al.</i>,  2004)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007) and EDMA (Palatinus <i>et al.</i>,
2012)'
;
_diffrn_ambient_temperature      80(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type
;
P11 beamline at PETRA III with Pilatus 6M detector (Kraft <i>et al.</i>,
2009)
;
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.56305
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43137
_diffrn_reflns_theta_full        19.745
_diffrn_reflns_theta_max         23.723
_diffrn_reflns_theta_min         1.180
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(XDS; Kabsch, 2010)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       prism
_exptl_crystal_F_000             589
_exptl_crystal_size_max          0.037
_exptl_crystal_size_mid          0.013
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7802
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0494P)^2^+2.9063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                7176
_reflns_number_total             7802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3128sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020632.cif.'
_cod_database_code               2020632
_cod_database_fobs_code          2020632
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.998
_shelx_hkl_checksum              97478
_shelx_res_checksum              96951