Uptake of one and two molecules of CO2 by the molybdate dianion: a soluble, molecular oxide model system for carbon dioxide fixation
Knopf, Ioana; Ono, Takashi; Temprado, Manuel; Tofan, Daniel; Cummins, Christopher C.; Chemical Science 5 (2014) 1772–; doi:10.1039/c4sc00132j

data_1514275
_publ_section_title
;
 Uptake of one and two molecules of CO2 by the molybdate dianion: a
 soluble, molecular oxide model system for carbon dioxide fixation
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1772
_journal_paper_doi               10.1039/c4sc00132j
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C82 H72 Mo N6 O8 P4'
_chemical_formula_weight         1489.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90.884(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7577(11)
_cell_length_b                   13.0244(13)
_cell_length_c                   25.943(3)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.63
_cell_measurement_theta_min      2.36
_cell_volume                     3634.5(7)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            203085
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.504
_diffrn_reflns_theta_min         1.570
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.737
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
; 
 Flack x determined using 10697 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         24166
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0423P)^2^+2.3576P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                23252
_reflns_number_total             24166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc00132j2.cif
_cod_data_source_block           x13097
_cod_original_cell_volume        3634.5(6)
_cod_database_code               1514275
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2012-9
_shelx_res_checksum              85695
_shelx_hkl_checksum              50537