Fully Oxidized and Mixed-Valent Polyoxomolybdates Structured by Bisphosphonates with Pendant Pyridine Groups: Synthesis, Structure and Photochromic Properties
Oms, Olivier; Benali, Tarik; Marrot, Jérome; Mialane, Pierre; Puget, Marin; Serier-Brault, Hélène; Deniard, Philippe; Dessapt, Rémi; Dolbecq, Anne; Inorganics 3 (2015) 279–; doi:10.3390/inorganics3020279

data_1520763
_publ_section_title
;
 Fully Oxidized and Mixed-Valent Polyoxomolybdates Structured by
 Bisphosphonates with Pendant Pyridine Groups: Synthesis, Structure and
 Photochromic Properties
;
_journal_issue                   2
_journal_name_full               Inorganics
_journal_page_first              279
_journal_paper_doi               10.3390/inorganics3020279
_journal_volume                  3
_journal_year                    2015
_chemical_formula_sum            'C20 H30 Mo6 N4 Na4 O48 P4'
_chemical_formula_weight         1885.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                103.992(2)
_cell_angle_beta                 95.5616(16)
_cell_angle_gamma                103.4068(14)
_cell_formula_units_Z            2
_cell_length_a                   9.0240(3)
_cell_length_b                   19.4282(6)
_cell_length_c                   21.1568(7)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.32
_cell_volume                     3454.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70048
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.005
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.186
_refine_diff_density_min         -3.486
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1110P)^2^+57.9125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10696
_reflns_number_total             12208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s1.cif
_cod_data_source_block           NaMo6(Ale-4Py)2
_cod_database_code               1520763
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.905
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'