Location controlled symmetry reduction: paradigm of an open metalloporphyrin framework based on the tetracarboxy porphyrin linker
Tripuramallu, Bharat Kumar; Titi, Hatem M.; Goswami, Soumyabrata; Phukan, Nithi; CrystEngComm 21 (2019) 5216–; doi:10.1039/C9CE01107B

data_7233296
_publ_section_title
;
 Location controlled symmetry reduction: paradigm of an open
 metalloporphyrin framework based on the tetracarboxy porphyrin linker
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5216
_journal_paper_doi               10.1039/C9CE01107B
_journal_volume                  21
_journal_year                    2019
_chemical_formula_sum            'C49 H25 Gd N4 O10 Zn'
_chemical_formula_weight         1052.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.467(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.903(3)
_cell_length_b                   16.7851(16)
_cell_length_c                   21.149(2)
_cell_measurement_reflns_used    4849
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.380
_cell_measurement_theta_min      1.668
_cell_volume                     6314.9(14)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26408
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        23.380
_diffrn_reflns_theta_max         23.380
_diffrn_reflns_theta_min         1.668
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.798
_exptl_transmission_factor_min   0.721
_refine_diff_density_max         4.348
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9115
_refine_ls_number_restraints     621
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1527P)^2^+14.5035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4849
_reflns_number_total             9115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01107b2.cif
_cod_data_source_block           s1
_cod_depositor_comments          'Adding full bibliography for 7233296.cif.'
_cod_original_cell_volume        6315.0(13)
_cod_database_code               7233296
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.892
_shelx_res_checksum              71114
_shelx_fab_checksum              81152