Crystal structure of <i>cis</i>-7,8-dihydroxy-5,10,15,20-tetraphenylchlorin and its zinc(II)–ethylenediamine complex
Chaudhri, Nivedita; Brückner, Christian; Zeller, Matthias; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022002729

data_2244055
_publ_section_title
;
 Crystal structure of
 <i>cis</i>-7,8-dihydroxy-5,10,15,20-tetraphenylchlorin and its
 zinc(II)--ethylenediamine complex
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022002729
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Zn (C44 H30 N4 O2)], C2 H8 N2, 0.136C H4 O'
_chemical_formula_moiety         'C46 H38 N6 O2 Zn, 0.136(C H4 O)'
_chemical_formula_sum            'C46.14 H38.54 N6 O2.14 Zn'
_chemical_formula_weight         776.57
_chemical_name_common
;
[Chlorin(2-)]zinc(II)--ethylenediamine--methanol (1/1/0.136)
;
_chemical_name_systematic
'[<i>cis</i>-7,8-Dihydroxy-5,10,15,20-tetraphenylchlorinato(2-)]zinc(II)--ethylenediamine--methanol (1/1/0.136)'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.1464(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1249(3)
_cell_length_b                   13.5400(4)
_cell_length_c                   27.0447(8)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.4169
_cell_measurement_theta_min      3.2815
_cell_volume                     3692.64(19)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX3 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b),
<i>ShelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonIII-C14 charge-integrating and
photon counting pixel array detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21319
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.470
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1618
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7551
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+1.8191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                7037
_reflns_number_total             7551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2044sup1.cif
_cod_data_source_block           2PhZn
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2244055
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.798
_shelx_hkl_checksum              85471
_shelx_res_checksum              9431
_cod_database_fobs_code 2244055