Binuclear molybdenum alkoxide as the versatile catalyst for the conversion of carbon dioxide
Chen, Jing-Huo; Deng, Cheng-Hua; Fang, Sheng; Ma, Jian-Gong; Cheng, Peng; Green Chemistry 20 (2018) 989–; doi:10.1039/C7GC03372A

data_7229844
_publ_section_title
;
 Binuclear molybdenum alkoxide as the versatile catalyst for the
 conversion of carbon dioxide
;
_journal_issue                   5
_journal_name_full               'Green Chemistry'
_journal_page_first              989
_journal_paper_doi               10.1039/C7GC03372A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C11 H5 O2'
_chemical_formula_sum            'C11 H5 O2'
_chemical_formula_weight         169.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-14 deposited with the CCDC.
2017-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.034(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.8398(8)
_cell_length_b                   6.201(3)
_cell_length_c                   35.222(7)
_cell_measurement_reflns_used    797
_cell_measurement_temperature    120(10)
_cell_measurement_theta_max      26.6590
_cell_measurement_theta_min      3.7160
_cell_volume                     838.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -34.00  27.00   1.00   26.25    --  -19.25  57.00  90.00   61
  2  \w     35.00  87.00   1.00   26.25    --   18.94 178.00-120.00   52
  3  \w    -80.00 -10.00   1.00   26.25    --  -19.25 -77.00-150.00   70
  4  \w     41.00  94.00   1.00   26.25    --   18.94-178.00  30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0321965000
_diffrn_orient_matrix_UB_12      0.0281107000
_diffrn_orient_matrix_UB_13      0.0191731000
_diffrn_orient_matrix_UB_21      0.1719717000
_diffrn_orient_matrix_UB_22      -0.0310447000
_diffrn_orient_matrix_UB_23      0.0051878000
_diffrn_orient_matrix_UB_31      0.0589104000
_diffrn_orient_matrix_UB_32      0.1064303000
_diffrn_orient_matrix_UB_33      -0.0034425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            3042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.988
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+1.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1221
_reflns_number_total             1490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7gc03372a2.cif
_cod_data_source_block           p161115c1
_cod_depositor_comments
'Adding full bibliography for 7229843--7229844.cif.'
_cod_original_cell_volume        838.6(4)
_cod_database_code               7229844
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N'
_chemical_oxdiff_usercomment     1,4BQS
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 O11, C9, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
O10 \\sim C9 \\sim O11: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C2(H2), C6(H6)
4.b :
 C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.996
_oxdiff_exptl_absorpt_empirical_full_min 0.495