Structural and coordination studies of "pearl oysterlike" porphyrins.
Halime, Zakaria; Lachkar, Mohammed; Roisnel, Thierry; Richard, Philippe; Boitrel, Bernard; Inorganic chemistry 46 (2007) 6338–6346; doi:10.1021/ic0703272

data_4339261
_publ_section_title
;
 Structural and coordination studies of &quot;pearl oysterlike&quot;
 porphyrins.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6338
_journal_page_last               6346
_journal_paper_doi               10.1021/ic0703272
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C90 H72 N8 O12 Zn, 2(C4 H8 O), 2(C2 H3 N)'
_chemical_formula_sum            'C102 H94 N10 O14 Zn'
_chemical_formula_weight         1749.26
_space_group_IT_number           14
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.9390(10)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            2
_cell_length_a                   14.7305(2)
_cell_length_b                   20.9723(4)
_cell_length_c                   15.4816(3)
_cell_measurement_reflns_used    10102
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1
_cell_volume                     4336.81(14)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens & al., 1999)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23385
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.75
_diffrn_standards_interval_count 0
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0693P)^2^+3.0352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                6179
_reflns_number_total             9892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0703272-file001.cif
_cod_data_source_block           1Zn(THF)2
_cod_original_cell_volume        4336.81(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4339261