Naphthylimido-Substituted Hexamolybdate: Preparation, Crystal Structures, Solvent Effects, and Optical Properties of Three Polymorphs
Jian Hao; Laurent Ruhlmann; Yulin Zhu; Qiang Li; Yongge Wei; Inorganic Chemistry 46 (2007) 4960–4967; doi:10.1021/ic070064b

data_4308090
_publ_section_title
;
Naphthylimido-Substituted Hexamolybdate: Preparation, Crystal Structures,
Solvent Effects, and Optical Properties of Three Polymorphs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4960
_journal_page_last               4967
_journal_paper_doi               10.1021/ic070064b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C43 H81 Mo6 N3 O18'
_chemical_formula_weight         1503.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.005(3)
_cell_length_b                   22.680(5)
_cell_length_c                   19.890(4)
_cell_measurement_reflns_used    41267
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      3.105
_cell_volume                     5678(2)
_computing_cell_refinement       'Rigaku RAPID AUTO Ver2.30'
_computing_data_collection       'Rigaku RAPID AUTO Ver2.30'
_computing_data_reduction        'Rigaku RAPID AUTO Ver2.30'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      288(2)
_diffrn_detector_area_resol_mean '100x100 micron'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46812
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.8767
_exptl_absorpt_correction_T_min  0.5513
_exptl_absorpt_correction_type   MULTI-SACAN
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.993
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         11109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                7157
_reflns_number_total             11109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070064b-file001.cif
_cod_data_source_block           test
_cod_database_code               4308090