Ferrocene Tethered Boramidinate Frustrated Lewis Pairs: Stepwise Capture of CO2 and CO
Esarte Palomero, Orhi; Jones, Richard A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00691J

data_7709871
_publ_section_title
;
 Ferrocene Tethered Boramidinate Frustrated Lewis Pairs: Stepwise Capture
 of CO2 and CO
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00691J
_journal_year                    2022
_chemical_formula_moiety         'C46 H28 B2 F20 Fe N4 O2'
_chemical_formula_sum            'C46 H28 B2 F20 Fe N4 O2'
_chemical_formula_weight         1126.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-30 deposited with the CCDC.	2022-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9212(3)
_cell_length_b                   10.11460(10)
_cell_length_c                   14.4015(2)
_cell_measurement_reflns_used    7939
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      75.5860
_cell_measurement_theta_min      4.5880
_cell_volume                     4501.48(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_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   -120.00  -1.00   1.00   15.00    --  -41.34 -19.00-150.00  119
  2  \w    -42.00  28.00   1.00   15.00    --  -41.34  38.00  30.00   70
  3  \w     37.00  93.00   1.00   15.00    --   41.34-125.00 -60.00   56
  4  \w     85.00 135.00   1.00   45.00    --  112.00  30.00  60.00   50
  5  \w     50.00 119.00   1.00   45.00    --  112.00 -61.00 -30.00   69
  6  \w     96.00 132.00   1.00   45.00    --  112.00  30.00 150.00   36
  7  \w    141.00 167.00   1.00   45.00    --  112.00 111.00   0.00   26
  8  \w     29.00 106.00   1.00   45.00    --  112.00 -94.00 -90.00   77
  9  \w    104.00 178.00   1.00   45.00    --  112.00 111.00 -30.00   74
 10  \w     32.00  84.00   1.00   45.00    --  112.00 -94.00 -30.00   52
 11  \w    149.00 177.00   1.00   45.00    --  112.00  30.00  30.00   28
 12  \w    136.00 174.00   1.00   45.00    --  112.00 111.00  60.00   38
 13  \w     41.00  67.00   1.00   45.00    --  112.00 -94.00-150.00   26
 14  \w     78.00 104.00   1.00   45.00    --  112.00 -94.00-150.00   26
 15  \w     89.00 116.00   1.00   45.00    --  112.00  30.00  30.00   27
 16  \w    142.00 177.00   1.00   45.00    --  112.00  30.00  60.00   35
 17  \w     33.00  79.00   1.00   45.00    --  112.00 -94.00   0.00   46
 18  \w     78.00 107.00   1.00   45.00    --  112.00 -94.00 -60.00   29
 19  \w     39.00 116.00   1.00   45.00    --  112.00 -45.00  30.00   77
 20  \w     68.00  94.00   1.00   45.00    --  112.00-111.00-180.00   26
 21  \w     29.00  30.00   1.00   45.00    --  112.00 -94.00 -60.00    1
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016301000
_diffrn_orient_matrix_UB_12      -0.0441247000
_diffrn_orient_matrix_UB_13      -0.1024366000
_diffrn_orient_matrix_UB_21      -0.0142704000
_diffrn_orient_matrix_UB_22      0.1400567000
_diffrn_orient_matrix_UB_23      -0.0298384000
_diffrn_orient_matrix_UB_31      0.0477437000
_diffrn_orient_matrix_UB_32      0.0403734000
_diffrn_orient_matrix_UB_33      -0.0085563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12442
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.801
_diffrn_reflns_theta_min         2.860
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.865
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       needle
_exptl_crystal_F_000             2256
_exptl_crystal_recrystallization_method
'Layering hexanes over dichloromethane solution of the compound'
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0829P)^2^+1.9081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4553
_reflns_number_total             4613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           tbupierscoabsz3
_cod_database_code               7709871
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C46H28F20B2Fe1N4O2
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
;
_shelx_res_checksum              723
_olex2_exptl_crystal_mounting_method
'Coated in paratone oil and mounted on a nylon loop'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.895
_oxdiff_exptl_absorpt_empirical_full_min 0.484