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_7709877
_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 O4, C H2 Cl2'
_chemical_formula_sum            'C47 H30 B2 Cl2 F20 Fe N4 O4'
_chemical_formula_weight         1243.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-01
_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                 115.732(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3630(3)
_cell_length_b                   25.0739(5)
_cell_length_c                   10.4150(3)
_cell_measurement_reflns_used    10741
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      75.4560
_cell_measurement_theta_min      3.4900
_cell_volume                     2437.88(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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      100.0(4)
_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 0.990
_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    -80.00  -2.00   1.00   17.50    --  -41.59 125.00  60.00   78
  2  \w   -111.00 -17.00   1.00   17.50    --  -41.59 -38.00-120.00   94
  3  \w   -115.00 -13.00   1.00   17.50    --  -41.59 -57.00   0.00  102
  4  \w   -102.00 -21.00   1.00   17.50    --  -41.59 -38.00 150.00   81
  5  \w     51.00  90.00   1.00   17.50    --   41.59-125.00 -30.00   39
  6  \w     37.00  64.00   1.00   50.00    --  112.00-111.00  30.00   27
  7  \w     49.00  76.00   1.00   50.00    --  112.00 -45.00 120.00   27
  8  \w     35.00 110.00   1.00   50.00    --  112.00 -94.00  60.00   75
  9  \w     36.00 113.00   1.00   50.00    --  112.00-111.00 -60.00   77
 10  \w    118.00 164.00   1.00   50.00    --  112.00 -15.00 -30.00   46
 11  \w     30.00 117.00   1.00   50.00    --  112.00 -15.00 -30.00   87
 12  \w     60.00 178.00   1.00   50.00    --  112.00  15.00   0.00  118
 13  \w     93.00 138.00   1.00   50.00    --  112.00 -45.00 120.00   45
 14  \w     40.00 133.00   1.00   50.00    --  112.00 -61.00 -90.00   93
 15  \w     79.00 113.00   1.00   50.00    --  112.00-111.00  30.00   34
 16  \w     44.00 132.00   1.00   50.00    --  112.00 -45.00  30.00   88
 17  \w     39.00 113.00   1.00   50.00    --  112.00-111.00-180.00   74
 18  \w     35.00 107.00   1.00   50.00    --  112.00 -94.00-150.00   72
 19  \w     68.00 161.00   1.00   50.00    --  112.00 -15.00 120.00   93
 20  \w     30.00  57.00   1.00   50.00    --  112.00 -15.00 120.00   27
;
_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      -0.0677012000
_diffrn_orient_matrix_UB_12      -0.0535171000
_diffrn_orient_matrix_UB_13      0.0107354000
_diffrn_orient_matrix_UB_21      -0.0345788000
_diffrn_orient_matrix_UB_22      -0.0122756000
_diffrn_orient_matrix_UB_23      -0.1565680000
_diffrn_orient_matrix_UB_31      0.1464481000
_diffrn_orient_matrix_UB_32      -0.0275913000
_diffrn_orient_matrix_UB_33      0.0483109000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19493
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.736
_diffrn_reflns_theta_min         3.525
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
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    1.693
_exptl_crystal_description       plate
_exptl_crystal_F_000             1244
_exptl_crystal_recrystallization_method
'Slow vapour diffusion of pentane into a dichloromethane solution'
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 3638 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         9626
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0645P)^2^+0.8062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                8916
_reflns_number_total             9626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           oepgfctbupiersco2
_cod_original_cell_volume        2437.88(13)
_cod_database_code               7709877
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C47H30B2N4Fe1F20O4Cl2
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.643
_reflns_odcompleteness_completeness 99.69
_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 Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C1(H1), C24(H24), C23(H23), C27(H27), C25(H25), C26(H26), C20(H20),
 C21(H21), C22(H22)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C6(H6A,H6B,H6C), C33(H33A,H33B,H33C), C5(H5A,H5B,H5C),
 C34(H34A,H34B,H34C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              65932
_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 1.936
_oxdiff_exptl_absorpt_empirical_full_min 0.667