Activation and functionalisation of carbon dioxide by bis-tris(pyrazolyl)borate-supported divalent samarium and trivalent lanthanide silylamide complexes.
Chowdhury, Tajrian; Wilson, Claire; Farnaby, Joy H.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11884–11894; doi:10.1039/d4dt01382d

data_7716447
_publ_section_title
;
 Activation and functionalisation of carbon dioxide by
 bis-tris(pyrazolyl)borate-supported divalent samarium and trivalent
 lanthanide silylamide complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11884
_journal_page_last               11894
_journal_paper_doi               10.1039/d4dt01382d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C21 H23 B2 N14 Y'
_chemical_formula_sum            'C21 H23 B2 N14 Y'
_chemical_formula_weight         582.06
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-04-12 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.332(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.007(3)
_cell_length_b                   9.3117(17)
_cell_length_c                   21.482(4)
_cell_measurement_reflns_used    1530
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.23
_cell_measurement_theta_min      3.15
_cell_volume                     2586.0(9)
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.378
_diffrn_measured_fraction_theta_max 0.352
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1446
_diffrn_reflns_av_unetI/netI     0.1373
_diffrn_reflns_Laue_measured_fraction_full 0.92
_diffrn_reflns_Laue_measured_fraction_max 0.92
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.394
_diffrn_reflns_theta_min         1.908
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_T_max  0.745375
_exptl_absorpt_correction_T_min  0.324899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1162 before and 0.0633 after correction.
 
For component 2:
 wR2(int) was 0.1434 before and 0.0652 after correction.
 
For component 3:
 wR2(int) was 0.1233 before and 0.0650 after correction.
 The Ratio of minimum to maximum transmission is 0.43.

Final HKLF 4 output contains 19829 reflections, Rint = 0.1446
 (5791 with I > 3sig(I), Rint = 0.1087)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4885
_refine_ls_number_restraints     407
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1180P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3296
_reflns_number_total             4885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01382d2.cif
_cod_data_source_block           Y_pz_YTp2pz
_cod_depositor_comments
'Adding full bibliography for 7716442--7716448.cif.'
_cod_database_code               7716447
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.696
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.439(10)
 0.369(4) 0.192(9)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 B2(H2A), B1(H1A)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C3(H3), C11(H11), C9(H9), C1(H1), C15(H15), C18(H18), C16(H16),
 C20(H20), C8(H8), C10(H10), C6(H6), C17(H17), C21(H21), C5(H5), C13(H13),
 C4(H4), C19(H19), C2(H2), C14(H14), C7(H7)
;
_shelx_res_checksum              79691
_olex2_submission_special_instructions 'No special instructions were received'