Carboxylate-Functionalized Phosphomolybdates: Ligand-Directed Conformations
Donghui Yang; Suzhi Li; Pengtao Ma; Jingping Wang; Jingyang Niu; Inorganic Chemistry 52 (2013) 8987–8992; doi:10.1021/ic401176j

data_4335618
_publ_section_title
;
 Carboxylate-Functionalized Phosphomolybdates: Ligand-Directed
 Conformations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8987
_journal_page_last               8992
_journal_paper_doi               10.1021/ic401176j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C21 H44 Mo6 N5 O34 P'
_chemical_formula_weight         1517.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.372(3)
_cell_angle_beta                 105.949(3)
_cell_angle_gamma                91.991(3)
_cell_formula_units_Z            2
_cell_length_a                   12.473(2)
_cell_length_b                   14.023(2)
_cell_length_c                   16.024(2)
_cell_measurement_reflns_used    1493
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.25
_cell_measurement_theta_min      2.74
_cell_volume                     2686.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13552
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.8424
_exptl_absorpt_correction_T_min  0.5753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       Block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.0045(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1217P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1958
_reflns_number_gt                6566
_reflns_number_total             9360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401176j_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2686.5(7)
_cod_database_code               4335618