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_4332803
_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         'C37 H69 N5 Mo6 O32 P0.50 '
_chemical_formula_sum            'C37 H69 Mo6 N5 O32 P0.5'
_chemical_formula_weight         1687.09
_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                102.682(13)
_cell_angle_beta                 91.732(17)
_cell_angle_gamma                105.289(16)
_cell_formula_units_Z            2
_cell_length_a                   14.241(6)
_cell_length_b                   14.617(5)
_cell_length_c                   14.878(6)
_cell_measurement_reflns_used    21881
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2902(2)
_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
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.037
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27848
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.550
_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    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1683.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.90
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     814
_refine_ls_number_reflns         9286
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.0066
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    9357.0500    13127.1000    4268.6200
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                9235
_reflns_number_total             13000
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic060857isup4.cif
_cod_data_source_block           '____pA'
_cod_original_cell_volume        2901.6(20)
_cod_original_formula_sum        'C37 H69 N5 Mo6 O32 P0.50 '
_cod_database_code               4332803