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_7709875
_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         'C68 H30 B4 F40 Fe N4'
_chemical_formula_sum            'C68 H30 B4 F40 Fe N4'
_chemical_formula_weight         1762.05
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_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                 98.190(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8703(3)
_cell_length_b                   13.4644(3)
_cell_length_c                   20.3086(4)
_cell_measurement_reflns_used    17697
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      75.5450
_cell_measurement_theta_min      3.9040
_cell_volume                     3754.06(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -66.00  30.00   1.00   12.00    --  -41.59  38.00  30.00   96
  2  \w    -93.00  -2.00   1.00   12.00    --  -41.59 125.00  30.00   91
  3  \w    -92.00  -6.00   1.00   12.00    --  -41.59 125.00 120.00   86
  4  \w   -107.00 -17.00   1.00   12.00    --  -41.59 -38.00-150.00   90
  5  \w     42.00  88.00   1.00   30.00    --  112.00-111.00  60.00   46
  6  \w     39.00 113.00   1.00   30.00    --  112.00-111.00 -30.00   74
  7  \w     75.00 144.00   1.00   30.00    --  112.00 -77.00 150.00   69
  8  \w     81.00 112.00   1.00   30.00    --  112.00-111.00-180.00   31
  9  \w    101.00 178.00   1.00   30.00    --  112.00 111.00  90.00   77
 10  \w     85.00 174.00   1.00   30.00    --  112.00  61.00-120.00   89
 11  \w     38.00 110.00   1.00   30.00    --  112.00-111.00  30.00   72
 12  \w     37.00  73.00   1.00   30.00    --  112.00-111.00-120.00   36
 13  \w     87.00 113.00   1.00   30.00    --  112.00-111.00-120.00   26
 14  \w     45.00 137.00   1.00   30.00    --  112.00 -61.00  60.00   92
 15  \w    127.00 178.00   1.00   30.00    --  112.00  45.00 150.00   51
 16  \w     90.00 116.00   1.00   30.00    --  112.00  45.00 150.00   26
 17  \w     86.00 175.00   1.00   30.00    --  112.00  45.00-180.00   89
 18  \w     37.00 113.00   1.00   30.00    --  112.00-111.00  90.00   76
 19  \w     84.00 162.00   1.00   30.00    --  112.00  61.00 -90.00   78
 20  \w     85.00 176.00   1.00   30.00    --  112.00  61.00-150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0956926000
_diffrn_orient_matrix_UB_12      0.0561933000
_diffrn_orient_matrix_UB_13      -0.0039537000
_diffrn_orient_matrix_UB_21      0.0242219000
_diffrn_orient_matrix_UB_22      -0.0730047000
_diffrn_orient_matrix_UB_23      -0.0537316000
_diffrn_orient_matrix_UB_31      -0.0533602000
_diffrn_orient_matrix_UB_32      0.0677807000
_diffrn_orient_matrix_UB_33      -0.0545600000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29331
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.718
_diffrn_reflns_theta_min         3.219
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.559
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_recrystallization_method
'Layering a concentrated dichloromethane solution with hexanes'
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.113
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         7750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0724
_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^)+(0.1322P)^2^+9.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7417
_reflns_number_total             7750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           oepgfcpiers_piersabs
_cod_database_code               7709875
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C68H30B4F40Fe1N4
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.336
_reflns_odcompleteness_completeness 99.79
_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), C32(H32), C33(H33), C31(H31), C34(H34)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              19764
_shelx_fab_checksum              44634
_olex2_exptl_crystal_mounting_method
'Coated in paratone oil an  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 2.143
_oxdiff_exptl_absorpt_empirical_full_min 0.507