Preparation of Nickel(II) 5,10,15,20-Tetraphenyl[1,2-c]pyrrolo-21-ethylcarboxyl-22-dipyrrylmethylporphyrin
ISHIMARU, Yoshihiro; KOBAYASHI, Yuta; FUJIHARA, Takashi; X-ray Structure Analysis Online 29 (2013) 37–; doi:10.2116/xraystruct.29.37

data_1551686
_publ_section_title
;
 Preparation of Nickel(II)
 5,10,15,20-Tetraphenyl[1,2-c]pyrrolo-21-ethylcarboxyl-22-dipyrrylmethylporphyrin
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              37
_journal_paper_doi               10.2116/xraystruct.29.37
_journal_volume                  29
_journal_year                    2013
_chemical_formula_sum            'C58 H41 N7 Ni O2'
_chemical_formula_weight         926.69
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.289(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.002(5)
_cell_length_b                   11.984(3)
_cell_length_c                   24.361(7)
_cell_measurement_reflns_used    5233
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.22
_cell_volume                     4960(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT and XPREP (Bruker, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'Bruker XCIF (Bruker, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51432
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS2008/1(Bruker,2008)
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The hexane and CHCl3 solvent molecule could not be resolved due to 
extensive disorder and their assumed presence was removed from the 
overall scattering by the PLATON SQUEEZE procedure [Spek (2009). 
Acta Cryst. D65, 148-155]. A total of 112 e was found in each cavity
(estimated volume 479 \%A^3^),corresponding to approximately one hexane 
and one CHCl3 molecules per cavity.
;
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                6229
_reflns_number_total             10137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            29_37_1.txt
_cod_data_source_block           fuji_maru_NiComplex
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 6524 2018-11-02 12:15:13Z antanas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1551686