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_7709872
_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         'C54 H46 B2 F20 Fe N6'
_chemical_formula_sum            'C54 H46 B2 F20 Fe N6'
_chemical_formula_weight         1236.44
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.77070(10)
_cell_length_b                   11.77070(10)
_cell_length_c                   38.8441(4)
_cell_measurement_reflns_used    21978
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      75.7360
_cell_measurement_theta_min      3.8560
_cell_volume                     5381.83(9)
_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      99.9(5)
_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 0.997
_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    -62.00  15.00   1.00   12.50    --  -41.59  38.00 150.00   77
  2  \w    -66.00  32.00   1.00   12.50    --  -41.59  38.00  30.00   98
  3  \w    -93.00  -5.00   1.00   12.50    --  -41.59 125.00 120.00   88
  4  \w   -107.00 -17.00   1.00   12.50    --  -41.59 -38.00-150.00   90
  5  \w     45.00  92.00   1.00   12.50    --   41.59-125.00  60.00   47
  6  \w     46.00 111.00   1.00   35.00    --  112.00-111.00 150.00   65
  7  \w     36.00 140.00   1.00   35.00    --  112.00 -30.00-150.00  104
  8  \w    106.00 138.00   1.00   35.00    --  112.00 -45.00 -30.00   32
  9  \w     54.00 139.00   1.00   35.00    --  112.00 -61.00-120.00   85
 10  \w     39.00 113.00   1.00   35.00    --  112.00-111.00 -90.00   74
 11  \w     42.00 109.00   1.00   35.00    --  112.00 -94.00 150.00   67
 12  \w     59.00 177.00   1.00   35.00    --  112.00  15.00  90.00  118
 13  \w     41.00 125.00   1.00   35.00    --  112.00 -45.00 120.00   84
 14  \w     45.00  76.00   1.00   35.00    --  112.00-111.00  90.00   31
 15  \w     88.00 113.00   1.00   35.00    --  112.00-111.00  90.00   25
 16  \w     39.00  64.00   1.00   35.00    --  112.00 -45.00 -30.00   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      -0.0605956000
_diffrn_orient_matrix_UB_12      0.1141393000
_diffrn_orient_matrix_UB_13      0.0062575000
_diffrn_orient_matrix_UB_21      -0.0840571000
_diffrn_orient_matrix_UB_22      -0.0593093000
_diffrn_orient_matrix_UB_23      0.0245220000
_diffrn_orient_matrix_UB_31      0.0798700000
_diffrn_orient_matrix_UB_32      0.0241988000
_diffrn_orient_matrix_UB_33      0.0305535000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            34806
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.765
_diffrn_reflns_theta_min         3.924
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69018
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_recrystallization_method
'Slow evaporation of dichloromethane solution'
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0091(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0704P)^2^+0.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.689
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                5426
_reflns_number_total             5566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           opegpierscntbuabs
_cod_original_cell_volume        5381.83(11)
_cod_database_code               7709872
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C54H46B2F20B2Fe1N6
_chemical_oxdiff_usercomment     'prism yellow'
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.621
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C25(H25), C24(H24), C27(H27), C26(H26)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C),
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              46685
_olex2_exptl_crystal_mounting_method
'Coated in paratone oil, 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 1.681
_oxdiff_exptl_absorpt_empirical_full_min 0.488