Crystal structure and photophysical properties of a novel polyoxomolybdate porphyrin
Chen, Wen-Tong; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620014461

data_2022274
_publ_section_title
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 Crystal structure and photophysical properties of a novel
 polyoxomolybdate porphyrin
;
_journal_coeditor_code           ZO3009
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620014461
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C48 H32 N4 O8) [Mo6 O19], 5H2 O'
_chemical_formula_moiety         'C48 H32 N4 O8 2+, Mo6 O19 2-, 5(H2 O)'
_chemical_formula_sum            'C48 H42 Mo6 N4 O32'
_chemical_formula_weight         1762.49
_chemical_melting_point          ?
_chemical_name_common            Mo6O19.H2TCPP.5H2O
_chemical_name_systematic
;5,10,15,20-Tetrakis(4-carboxyphenyl)-21<i>H</i>,22<i>H</i>,23<i>H</i>,
\24<i>H</i>-porphine(2+) hexamolybdate(VI) pentahydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3159(8)
_cell_length_b                   15.0183(5)
_cell_length_c                   19.6537(10)
_cell_measurement_reflns_used    3496
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2010
_cell_measurement_theta_min      3.5620
_cell_volume                     5701.4(4)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1787
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.1623
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15930
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.733
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         5129
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.2046
_refine_ls_R_factor_gt           0.0922
_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^)+(0.0397P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                2187
_reflns_number_total             5129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3009sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
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_cod_database_code               2022274
_shelx_hkl_checksum              84699
_shelx_res_checksum              1100
_cod_database_fobs_code 2022274