Organoimido-Derivatized Hexamolybdates with a Remote Carboxyl Group: Syntheses and Structural Characterizations
Guohui Sima; Qiang Li; Yi Zhu; Chunlin Lv; Rao Naumaan Nasim Khan; Jian Hao; Jin Zhang; Yongge Wei; Inorganic Chemistry 52 (2013) 6551–6558; doi:10.1021/ic4005278

data_4335092
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
P. R. China
;
_publ_contact_author_email
'yonggewei@mail.tsinghua.edu.cn, jinjin_eva@163.com'
_publ_contact_author_name        'Yongge Wei, Jin Zhang'
_publ_section_title
;
 Organoimido-Derivatized Hexamolybdates with a Remote Carboxyl Group:
 Syntheses and Structural Characterizations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6551
_journal_page_last               6558
_journal_paper_doi               10.1021/ic4005278
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C42 H83.5 Mo6 N3.5 O20.5'
_chemical_formula_weight         1541.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.9827(6)
_cell_length_b                   24.1195(10)
_cell_length_c                   23.8593(7)
_cell_measurement_reflns_used    10765
_cell_measurement_temperature    102.2
_cell_measurement_theta_max      29.2215
_cell_measurement_theta_min      3.0622
_cell_volume                     11499.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      102.2
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w 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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38961
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.6892
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             6208
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         11300
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0481
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                8456
_reflns_number_total             11300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4005278_si_002_2.cif
_cod_data_source_block           compound1
_cod_original_formula_sum        'C42 H83.50 Mo6 N3.50 O20.50'
_cod_database_code               4335092