Ameliorated synthetic methodology for crystalline lanthanoid‒metalloporphyrin open frameworks based on a multitopic octacarboxy-porphyrin scaffold: structural, gas sorption and photophysical properties
Tripuramallu, Bharat Kumar; Titi, Hatem M.; Roy, Sadipan; Verma, Roli; Goldberg, Israel; CrystEngComm 18 (2016) 515–; doi:10.1039/C5CE02048D

data_7223239
_publ_section_title
;
 Ameliorated synthetic methodology for crystalline
 lanthanoid--metalloporphyrin open frameworks based on a multitopic
 octacarboxy-porphyrin scaffold: structural, gas sorption and
 photophysical properties
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              515
_journal_paper_doi               10.1039/C5CE02048D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C52 H30 N4 Na2 O21 Sm2 Zn'
_chemical_formula_sum            'C52 H30 N4 Na2 O21 Sm2 Zn'
_chemical_formula_weight         1458.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.108(4)
_cell_length_b                   29.418(3)
_cell_length_c                   12.9723(18)
_cell_measurement_reflns_used    4794
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      1.38
_cell_volume                     10345(2)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_unetI/netI     0.1556
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19423
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.090
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_min         1.384
_diffrn_source                   'ImuS micro-focus'
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.937
_exptl_crystal_description       prism
_exptl_crystal_F_000             2856
_exptl_crystal_recrystallization_method solvothermal
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;
 Numerous molecules of severely disordered DMF (+ water) solvent.
;
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1740
_reflns_number_total             4794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02048d2.cif
_cod_data_source_block           bkt16sq
_cod_depositor_comments
'Adding full bibliography for 7223238--7223241.cif.'
_cod_database_code               7223239
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.828