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_7709868
_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 H60 B2 Fe N4'
_chemical_formula_sum            'C46 H60 B2 Fe N4'
_chemical_formula_weight         746.45
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-31
_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                 101.017(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6596(2)
_cell_length_b                   7.8100(2)
_cell_length_c                   22.5086(4)
_cell_measurement_reflns_used    8720
_cell_measurement_temperature    100.03(10)
_cell_measurement_theta_max      75.5330
_cell_measurement_theta_min      3.8320
_cell_volume                     2011.89(7)
_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      100.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -68.00  25.00   1.00    5.00    --  -41.34  57.00-120.00   93
  2  \w   -112.00 -11.00   1.00    5.00    --  -41.34 -77.00  90.00  101
  3  \w    -63.00 -15.00   1.00    5.00    --  -41.34 125.00 -30.00   48
  4  \w    135.00 169.00   1.00   11.00    --  112.00  45.00   0.00   34
  5  \w     52.00 107.00   1.00   11.00    --  112.00 -30.00-180.00   55
  6  \w    115.00 140.00   1.00   11.00    --  112.00 -30.00-180.00   25
  7  \w     72.00 109.00   1.00   11.00    --  112.00 -94.00 120.00   37
  8  \w     37.00 137.00   1.00   11.00    --  112.00 -77.00 -30.00  100
  9  \w     84.00 173.00   1.00   11.00    --  112.00  61.00  90.00   89
 10  \w     43.00  77.00   1.00   11.00    --  112.00 -61.00-150.00   34
 11  \w    110.00 136.00   1.00   11.00    --  112.00 -61.00-150.00   26
 12  \w     32.00 105.00   1.00   11.00    --  112.00 -94.00 150.00   73
 13  \w     65.00  91.00   1.00   11.00    --  112.00 -30.00  90.00   26
 14  \w    105.00 138.00   1.00   11.00    --  112.00 -30.00  90.00   33
 15  \w     50.00  75.00   1.00   11.00    --  112.00 -61.00-180.00   25
 16  \w     30.00  55.00   1.00   11.00    --  112.00 -94.00-150.00   25
 17  \w     90.00 139.00   1.00   11.00    --  112.00 -61.00-180.00   49
 18  \w     40.00  66.00   1.00   11.00    --  112.00 -94.00  30.00   26
 19  \w     36.00  62.00   1.00   11.00    --  112.00 -94.00 120.00   26
 20  \w     82.00 108.00   1.00   11.00    --  112.00  15.00-150.00   26
 21  \w    117.00 165.00   1.00   11.00    --  112.00  15.00-150.00   48
 22  \w     66.00  95.00   1.00   11.00    --  112.00-111.00-150.00   29
 23  \w     47.00  74.00   1.00   11.00    --  112.00-111.00  90.00   27
 24  \w    120.00 147.00   1.00   11.00    --  112.00 178.00 -30.00   27
 25  \w    109.00 139.00   1.00   11.00    --  112.00 -30.00  30.00   30
 26  \w    103.00 128.00   1.00   11.00    --  112.00  45.00   0.00   25
;
_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      -0.0277015000
_diffrn_orient_matrix_UB_12      -0.1650465000
_diffrn_orient_matrix_UB_13      -0.0374630000
_diffrn_orient_matrix_UB_21      0.1317330000
_diffrn_orient_matrix_UB_22      -0.0336016000
_diffrn_orient_matrix_UB_23      0.0051239000
_diffrn_orient_matrix_UB_31      0.0014141000
_diffrn_orient_matrix_UB_32      -0.1025392000
_diffrn_orient_matrix_UB_33      0.0586083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12727
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.657
_diffrn_reflns_theta_min         3.862
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21196
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       irregular
_exptl_crystal_F_000             800
_exptl_crystal_recrystallization_method
'Toluene solution layered with hexanes'
_exptl_crystal_size_max          0.732
_exptl_crystal_size_mid          0.709
_exptl_crystal_size_min          0.343
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0522
_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^)+(0.1035P)^2^+0.7480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4021
_reflns_number_total             4166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           mes9bbn_3abs
_cod_database_code               7709868
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C46H60B2N4Fe1
_reflns_odcompleteness_completeness 98.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     76.55
_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:
 C20(H20), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C22(H22A,H22B), C21(H21A,H21B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C13(H13), C4(H4), C5(H5), C2(H2), C3(H3)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              25175
_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 2.379
_oxdiff_exptl_absorpt_empirical_full_min 0.543