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_7709878
_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         'C56 H29 B3 F30 Fe N4'
_chemical_formula_sum            'C56 H29 B3 F30 Fe N4'
_chemical_formula_weight         1416.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-23
_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                100.918(3)
_cell_angle_beta                 100.128(4)
_cell_angle_gamma                103.954(4)
_cell_formula_units_Z            2
_cell_length_a                   12.1902(6)
_cell_length_b                   15.3611(6)
_cell_length_c                   17.1353(5)
_cell_measurement_reflns_used    13172
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      75.5060
_cell_measurement_theta_min      4.8620
_cell_volume                     2973.9(2)
_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(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.964
_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    -65.00  20.00   1.00   12.50    --  -41.59  38.00 -60.00   85
  2  \w    -66.00  31.00   1.00   12.50    --  -41.59  57.00  30.00   97
  3  \w    -69.00  29.00   1.00   12.50    --  -41.59  77.00 150.00   98
  4  \w     58.00 112.00   1.00   12.50    --   41.59  57.00 120.00   54
  5  \w     13.00  55.00   1.00   12.50    --   41.59  57.00 120.00   42
  6  \w     49.00  96.00   1.00   12.50    --   41.59-125.00 -30.00   47
  7  \w     37.00 113.00   1.00   27.50    --  112.00-111.00 -30.00   76
  8  \w     61.00 150.00   1.00   27.50    --  112.00 178.00   0.00   89
  9  \w    103.00 176.00   1.00   27.50    --  112.00 111.00 -30.00   73
 10  \w     48.00 136.00   1.00   27.50    --  112.00 -77.00 -37.00   88
 11  \w     36.00 113.00   1.00   27.50    --  112.00-111.00-150.00   77
 12  \w     36.00  62.00   1.00   27.50    --  112.00-111.00 120.00   26
 13  \w    103.00 172.00   1.00   27.50    --  112.00 111.00   0.00   69
 14  \w     88.00 178.00   1.00   27.50    --  112.00  45.00 150.00   90
 15  \w     58.00 143.00   1.00   27.50    --  112.00 178.00-120.00   85
 16  \w     77.00 113.00   1.00   27.50    --  112.00-111.00 120.00   36
 17  \w     86.00 121.00   1.00   27.50    --  112.00  30.00  60.00   35
 18  \w    134.00 162.00   1.00   27.50    --  112.00  30.00  60.00   28
 19  \w     40.00 138.00   1.00   27.50    --  112.00 -45.00 -60.00   98
 20  \w     79.00 174.00   1.00   27.50    --  112.00  77.00  90.00   95
;
_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      0.0550403000
_diffrn_orient_matrix_UB_12      0.0210227000
_diffrn_orient_matrix_UB_13      -0.0711535000
_diffrn_orient_matrix_UB_21      -0.1038106000
_diffrn_orient_matrix_UB_22      0.0333274000
_diffrn_orient_matrix_UB_23      -0.0342683000
_diffrn_orient_matrix_UB_31      0.0641852000
_diffrn_orient_matrix_UB_32      0.0989665000
_diffrn_orient_matrix_UB_33      0.0512407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.668
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.283
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88168
_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    1.581
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'From toluene/pentane mixture at room temperature'
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         12106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0891P)^2^+0.3927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10921
_reflns_number_total             12106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           fctbupiers3abs
_cod_original_cell_volume        2973.8(2)
_cod_database_code               7709878
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C56H29B3F30FeN4
_reflns_odcompleteness_completeness 98.93
_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:
 C34(H34), C35(H35), C1(H1), C31(H31), C36(H36), C33(H33), C37(H37), C38(H38),
 C32(H32)
2.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C5(H5A,H5B,
 H5C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              20708
_shelx_fab_checksum              71214
_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 4.945
_oxdiff_exptl_absorpt_empirical_full_min 0.612