Mo- and W-Based Organic Nanostructures Prepared from Bulk Crystal Isomorphs Consisted of [(CH3CH2)3NH)]2[MO2(C14H6O4)2] (M = Mo, W)
B. Zhang; S. Z. Du; X. M. Lu; G. Wang; J. Fen; Inorganic Chemistry 52 (2013) 9470–9478; doi:10.1021/ic401125e

data_4335748
_publ_section_title
;
 Mo- and W-Based Organic Nanostructures Prepared from Bulk Crystal
 Isomorphs Consisted of [(CH3CH2)3NH)]2[MO2(C14H6O4)2] (M = Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9470
_journal_page_last               9478
_journal_paper_doi               10.1021/ic401125e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C40 H44 N2 O10 W'
_chemical_formula_weight         896.62
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.2330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.215(3)
_cell_length_b                   10.2110(10)
_cell_length_c                   13.5221(12)
_cell_measurement_reflns_used    4714
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.118
_cell_measurement_theta_min      2.635
_cell_volume                     3751.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9296
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    3.140
_exptl_absorpt_correction_T_max  0.4734
_exptl_absorpt_correction_T_min  0.4062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.335
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.349
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+4.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                2885
_reflns_number_total             3300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401125e_si_002.cif
_cod_data_source_block           120328b
_cod_database_code               4335748