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_4332800
_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         'C22 H42 N2 Mo6 O28 P0.50 '
_chemical_formula_sum            'C22 H42 Mo6 N2 O28 P0.5'
_chemical_formula_weight         1373.70
_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                82.65(8)
_cell_angle_beta                 68.75(9)
_cell_angle_gamma                65.81(9)
_cell_formula_units_Z            2
_cell_length_a                   12.07(4)
_cell_length_b                   13.15(3)
_cell_length_c                   14.45(4)
_cell_measurement_reflns_used    8824
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     1949(10)
_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    'DIRDIF99 (PATTY)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_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  0.119
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17719
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_exptl_absorpt_coefficient_mu    1.991
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1343.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.30
_refine_diff_density_min         -2.01
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     589
_refine_ls_number_reflns         5898
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.0114
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    2614.5300    3573.8800    1124.2100
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                1867
_reflns_number_total             8417
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic060857isup1.cif
_cod_data_source_block           '_Akutagawa'
_cod_original_cell_volume        1949(9)
_cod_original_formula_sum        'C22 H42 N2 Mo6 O28 P0.50 '
_cod_database_code               4332800