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_7709867
_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         'C38 H56 B2 Fe N4 O4'
_chemical_formula_sum            'C38 H56 B2 Fe N4 O4'
_chemical_formula_weight         710.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 103.831(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3039(13)
_cell_length_b                   6.8633(5)
_cell_length_c                   17.4316(15)
_cell_measurement_reflns_used    2431
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      75.0800
_cell_measurement_theta_min      2.9470
_cell_volume                     1777.8(3)
_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      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_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   -112.00 -15.00   1.00   15.00    --  -39.34 -38.00   0.00   97
  2  \w    -67.00 -13.00   1.00   15.00    --  -39.34  57.00-180.00   54
  3  \w     57.00 101.00   1.00   15.00    --   39.34 178.00 -30.00   44
  4  \w    -36.00  41.00   1.00   15.00    --   39.34 -77.00 -60.00   77
  5  \w     41.00 141.00   1.00   30.00    --  112.00 -61.00-180.00  100
  6  \w     83.00 138.00   1.00   30.00    --  112.00  61.00  90.00   55
  7  \w     82.00 132.00   1.00   30.00    --  112.00 -45.00 -60.00   50
  8  \w     84.00 113.00   1.00   30.00    --  112.00-111.00 150.00   29
  9  \w     36.00  63.00   1.00   30.00    --  112.00-111.00 150.00   27
 10  \w     84.00 171.00   1.00   30.00    --  112.00  30.00 -60.00   87
 11  \w     79.00 166.00   1.00   30.00    --  112.00  77.00 -30.00   87
 12  \w    153.00 178.00   1.00   30.00    --  112.00  61.00  90.00   25
 13  \w    109.00 178.00   1.00   30.00    --  112.00 111.00 -60.00   69
;
_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      -0.0621138000
_diffrn_orient_matrix_UB_12      -0.0128569000
_diffrn_orient_matrix_UB_13      0.0575628000
_diffrn_orient_matrix_UB_21      0.0534744000
_diffrn_orient_matrix_UB_22      0.1654206000
_diffrn_orient_matrix_UB_23      0.0500128000
_diffrn_orient_matrix_UB_31      -0.0634916000
_diffrn_orient_matrix_UB_32      0.1510925000
_diffrn_orient_matrix_UB_33      -0.0497237000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6663
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.667
_diffrn_reflns_theta_min         3.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25397
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_recrystallization_method
'Crystallized from a toluene solution under CO2 atmosphere'
_exptl_crystal_size_max          0.548
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1117P)^2^+2.5232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2940
_reflns_number_total             3597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           opegfctbu9bbnco2abs
_cod_database_code               7709867
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Fe1N4B2O4C38H56
_reflns_odcompleteness_completeness 98.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C12(H12A,H12B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
 C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C2(H2), C17(H17), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              67372
_shelx_fab_checksum              97335
_olex2_exptl_crystal_mounting_method
'Mounted on a nylon loop, coated in paratone oil'
_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 2.343
_oxdiff_exptl_absorpt_empirical_full_min 0.520