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_7716443
_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         'C38 H40 B4 N24 O4 Sm2'
_chemical_formula_sum            'C38 H40 B4 N24 O4 Sm2'
_chemical_formula_weight         1240.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-14 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9732(6)
_cell_length_b                   28.6287(8)
_cell_length_c                   21.4608(6)
_cell_measurement_reflns_used    17316
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.0050
_cell_measurement_theta_min      1.4840
_cell_volume                     12885.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 180.00   0.20    0.20   0.00   0.00   0.00    --   900
  2  \w   -145.00  25.00   0.20    0.20    --   30.00   0.00   0.00  850
  3  \w   -145.00  25.00   0.20    0.20    --   30.00   0.00 120.00  850
  4  \w   -145.00  25.00   0.20    0.20    --   30.00   0.00 240.00  850
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0323682500
_diffrn_orient_matrix_UB_12      -0.0039042000
_diffrn_orient_matrix_UB_13      -0.0018900500
_diffrn_orient_matrix_UB_21      0.0039588500
_diffrn_orient_matrix_UB_22      -0.0100231000
_diffrn_orient_matrix_UB_23      -0.0289426500
_diffrn_orient_matrix_UB_31      0.0040154500
_diffrn_orient_matrix_UB_32      -0.0215103000
_diffrn_orient_matrix_UB_33      0.0137762500
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54122
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         29.476
_diffrn_reflns_theta_min         1.486
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.558
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         9847
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1487
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7474
_reflns_number_total             9847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01382d2.cif
_cod_data_source_block           2_Sm_SmTp2_2_u_C2O4
_cod_depositor_comments
'Adding full bibliography for 7716442--7716448.cif.'
_cod_database_code               7716443
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H40B4N24O4Sm2
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.72(3)
 0.28(3)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C12(H12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43649
_shelx_fab_checksum              41687
_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 3.780
_oxdiff_exptl_absorpt_empirical_full_min 0.466