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_1520765
_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            'C32 H102.5 Mo8 N14 O53.25 P4'
_chemical_formula_weight         2427.18
_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                97.443(5)
_cell_angle_beta                 95.464(5)
_cell_angle_gamma                107.430(5)
_cell_formula_units_Z            4
_cell_length_a                   17.6023(19)
_cell_length_b                   22.134(2)
_cell_length_c                   28.323(3)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      2.45
_cell_volume                     10334.2(19)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            428822
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.9181
_exptl_absorpt_correction_T_min  0.7804
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4858
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.048
_refine_diff_density_min         -2.222
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2119
_refine_ls_number_reflns         36283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+261.6858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2719
_refine_ls_wR_factor_ref         0.2820
_reflns_number_gt                28875
_reflns_number_total             36283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            s1.cif
_cod_data_source_block           NH4Mo6(AlePy2Mo)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/MDPI/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_cell_volume        10333.9(19)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32 H102.50 Mo8 N14 O53.25 P4'
_cod_database_code               1520765