Formation ofp-Phenylenediamine−Crown Ether−[PMo12O40]4-Salts
Akutagawa, Tomoyuki; Endo, Daigoro; Imai, Hiroyuki; Noro, Shin-ichiro; Cronin, Leroy; Nakamura, Takayoshi; Inorganic Chemistry 45 (2006) 8628–8637; doi:10.1021/ic060857i

data_4332802
_publ_section_title
;
 Formation ofp-Phenylenediamine&#x2212;Crown
 Ether&#x2212;[PMo12O40]4-Salts
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8628
_journal_page_last               8637
_journal_paper_doi               10.1021/ic060857i
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C64 H116 N8 Mo12 O60 P '
_chemical_formula_sum            'C64 H116 Mo12 N8 O60 P'
_chemical_formula_weight         3139.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                65.13(6)
_cell_angle_beta                 64.74(6)
_cell_angle_gamma                67.12(6)
_cell_formula_units_Z            1
_cell_length_a                   13.74(3)
_cell_length_b                   14.52(2)
_cell_length_c                   16.26(3)
_cell_measurement_reflns_used    31583
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2574(8)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40485
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1555.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.65
_refine_diff_density_min         -1.88
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     763
_refine_ls_number_reflns         22278
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.0431
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    33619.3000    47196.6000    15118.3000
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                22278
_reflns_number_total             11600
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic060857isup3.cif
_cod_data_source_block           '_Akutagawa'
_cod_original_cell_volume        2573(8)
_cod_original_formula_sum        'C64 H116 N8 Mo12 O60 P '
_cod_database_code               4332802