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_7709873
_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 O3, C H2 Cl2'
_chemical_formula_sum            'C47 H30 B2 Cl2 F20 Fe N4 O3'
_chemical_formula_weight         1227.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-27
_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                 99.229(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2365(9)
_cell_length_b                   10.0331(5)
_cell_length_c                   27.3093(15)
_cell_measurement_reflns_used    4592
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      74.4170
_cell_measurement_theta_min      4.9060
_cell_volume                     4932.1(4)
_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(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_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    -69.00  26.00   1.00   37.50    --  -41.34  57.00 -90.00   95
  2  \w   -115.00 -22.00   1.00   37.50    --  -41.34 -39.00 109.00   93
  3  \w     27.00  97.00   1.00   37.50    --   41.34-125.00 120.00   70
  4  \w     85.00 178.00   1.00  110.00    --  112.00  30.00-120.00   93
  5  \w    101.00 139.00   1.00  110.00    --  112.00 -61.00  60.00   38
  6  \w     40.00  93.00   1.00  110.00    --  112.00 -61.00  60.00   53
  7  \w    115.00 140.00   1.00  110.00    --  112.00 -30.00 -60.00   25
  8  \w     37.00 101.00   1.00  110.00    --  112.00 -30.00 -60.00   64
  9  \w     42.00 113.00   1.00  110.00    --  112.00-111.00   0.00   71
 10  \w    116.00 171.00   1.00  110.00    --  112.00 111.00-180.00   55
 11  \w     60.00 176.00   1.00  110.00    --  112.00  15.00-180.00  116
;
_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      -0.0472467000
_diffrn_orient_matrix_UB_12      0.0758518000
_diffrn_orient_matrix_UB_13      0.0327636000
_diffrn_orient_matrix_UB_21      0.0676374000
_diffrn_orient_matrix_UB_22      0.0085268000
_diffrn_orient_matrix_UB_23      0.0416532000
_diffrn_orient_matrix_UB_31      0.0226044000
_diffrn_orient_matrix_UB_32      0.1332782000
_diffrn_orient_matrix_UB_33      -0.0214223000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10692
_diffrn_reflns_point_group_measured_fraction_full 0.719
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.796
_diffrn_reflns_theta_min         3.279
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2456
_exptl_crystal_recrystallization_method
'Slow vapour diffusiuon of pentane into dichloromethane solution'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.022(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         7037
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0918
_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^)+(0.1785P)^2^+12.4226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2478
_refine_ls_wR_factor_ref         0.2597
_reflns_Friedel_coverage         0.409
_reflns_Friedel_fraction_full    0.441
_reflns_Friedel_fraction_max     0.399
_reflns_number_gt                6375
_reflns_number_total             7037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           oepgfcpierstbuco2cofacesabs
_cod_database_code               7709873
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C47H30B2F20Fe1N4O3Cl2
_reflns_odcompleteness_completeness 98.61
_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:
 C1(H1), C3(H3), C29(H29), C28(H28), C27(H27), C23(H23), C22(H22), C24(H24),
 C26(H26), C25(H25)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C),
 C34(H34A,H34B,H34C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              20255
_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 3.779
_oxdiff_exptl_absorpt_empirical_full_min 0.598