Tuning the Dimensionality of Polyoxometalate-Based Materials by Using a Mixture of Ligands
Rousseau, Guillaume; Rodriguez-Albelo, Luisa Marleny; Salomon, William; Mialane, Pierre; Marrot, Jérôme; Doungmene, Floriant; Mbomekallé, Israël-Martyr; de Oliveira, Pedro; Dolbecq, Anne; Crystal Growth & Design 15 (2015) 449–; doi:10.1021/cg501524a

data_4512470
_publ_section_title
;
 Tuning the Dimensionality of Polyoxometalate-Based Materials by Using a
 Mixture of Ligands
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              449
_journal_paper_doi               10.1021/cg501524a
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C138 H258 Mo24 N6 O98 P2 Zn8'
_chemical_formula_weight         6456.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.3420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6854(9)
_cell_length_b                   29.7276(11)
_cell_length_c                   34.8286(14)
_cell_measurement_reflns_used    78692
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.33
_cell_measurement_theta_min      1.26
_cell_volume                     22315.0(15)
_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      293(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            173126
_diffrn_reflns_theta_full        30.33
_diffrn_reflns_theta_max         30.33
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    2.236
_exptl_absorpt_correction_T_max  0.8964
_exptl_absorpt_correction_T_min  0.8073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'G. M. Sheldrick, SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             12760
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2261
_refine_ls_number_reflns         65876
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1280
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.121
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+149.1218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                39996
_reflns_number_total             65876
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg501524a_si_003.cif
_cod_data_source_block           epsilon2(biphen)3
_cod_depositor_comments
'Adding full bibliography for 4512470--4512473.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4512470