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_1520764
_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 K3.5 Mo6 N4 Na0.5 O45.5 P4'
_chemical_formula_weight         1902.34
_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                76.1880(10)
_cell_angle_beta                 69.5900(10)
_cell_angle_gamma                76.6690(10)
_cell_formula_units_Z            4
_cell_length_a                   17.9501(5)
_cell_length_b                   19.4745(4)
_cell_length_c                   19.8487(5)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.34
_cell_volume                     6231.6(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            227315
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.051
_diffrn_reflns_theta_min         1.091
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.559
_refine_diff_density_min         -2.535
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1558
_refine_ls_number_reflns         36431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0904P)^2^+41.6688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1649
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28528
_reflns_number_total             36431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s1.cif
_cod_data_source_block           NaKMo6(Ale-4Py)2
_cod_original_formula_sum        'C20 H30 K3.50 Mo6 N4 Na0.50 O45.50 P4'
_cod_database_code               1520764
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.643
_shelx_estimated_absorpt_t_max   0.938
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'