Chain length effect in the functionalization of polyoxometalates with α,ω-alkyldiphosphonates
Liu, Zhiwei; Wang, Wei; Tang, Jinkui; Li, Weiqi; Yin, Weiye; Fang, Xikui; Chemical Communications  (2019) –; doi:10.1039/C9CC02854D

data_7123434
_publ_section_title
;
 Chain length effect in the functionalization of polyoxometalates with
 \a,\w-alkyldiphosphonates
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02854D
_journal_year                    2019
_chemical_formula_sum            'C54 H248 Mn12 N20 Na2 O196 P8 W38'
_chemical_formula_weight         12254.03
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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-2013
_audit_update_record
;
2018-01-02 deposited with the CCDC.    2019-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5062(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.5337(5)
_cell_length_b                   27.5478(4)
_cell_length_c                   47.9165(12)
_cell_measurement_reflns_used    11930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.74
_cell_measurement_theta_min      2.15
_cell_volume                     50629.6(16)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.1528
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            122401
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.703
_diffrn_reflns_theta_min         2.907
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    17.920
_exptl_absorpt_correction_T_max  0.8021
_exptl_absorpt_correction_T_min  0.6305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS, 2006/1'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             44272
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         5.346
_refine_diff_density_min         -4.028
_refine_diff_density_rms         0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1590
_refine_ls_number_reflns         56996
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.2106
_refine_ls_R_factor_gt           0.1356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+15961.5771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2412
_refine_ls_wR_factor_ref         0.2769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32413
_reflns_number_total             56996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02854d2.cif
_cod_data_source_block           C5-lzw
_cod_original_cell_volume        50629.5(16)
_cod_database_code               7123434
_shelx_estimated_absorpt_t_min   0.222
_shelx_estimated_absorpt_t_max   0.413