Bifunctional silanol-based HBD catalysts for CO2 fixation into cyclic carbonates
Perez-Perez, Jovana; Hernández-Balderas, Uvaldo; Martínez-Otero, Diego; Jancik, Vojtech; New Journal of Chemistry 43 (2019) 18525–18533; doi:10.1039/C9NJ04840E

data_7058966
_publ_section_title
;
 Bifunctional silanol-based HBD catalysts for CO2 fixation into cyclic
 carbonates
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18525
_journal_page_last               18533
_journal_paper_doi               10.1039/C9NJ04840E
_journal_volume                  43
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H39 N2 O4 Si, I'
_chemical_formula_sum            'C18 H39 I N2 O4 Si'
_chemical_formula_weight         502.50
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-19 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.6051(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1990(6)
_cell_length_b                   10.1509(6)
_cell_length_c                   13.4605(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.30
_cell_volume                     1210.58(13)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21402
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.441
_diffrn_reflns_theta_min         2.299
_diffrn_source                   'Incoatec ImuS'
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       Prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.468
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
; 
 Flack x determined using 2457 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         5518
_refine_ls_number_restraints     1308
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.0286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5369
_reflns_number_total             5518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04840e2.cif
_cod_data_source_block           Comp_Rac13
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7058966
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.561
_shelx_estimated_absorpt_t_max   0.795
_shelx_res_checksum              4823