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_7709866
_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         'C16 H6 F24 O6 Zn'
_chemical_formula_sum            'C16 H6 F24 O6 Zn'
_chemical_formula_weight         815.58
_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   difmap
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc286fwt
_audit_creation_date             2020-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-22 deposited with the CCDC.	2022-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                72.590(9)
_cell_angle_beta                 86.231(9)
_cell_angle_gamma                88.879(10)
_cell_formula_units_Z            1
_cell_length_a                   5.1723(8)
_cell_length_b                   10.8211(12)
_cell_length_c                   11.3985(9)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    100.04(11)
_cell_measurement_theta_max      72.6560
_cell_measurement_theta_min      4.0240
_cell_volume                     607.43(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_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_temperature      100.04(11)
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.983
_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  32.00   1.00   10.00    --  -41.59  57.00   0.00  101
  2  \w    -63.00  33.00   1.00   10.00    --  -41.59  38.00 -90.00   96
  3  \w    -74.00  26.00   1.00   10.00    --  -41.59  77.00 120.00  100
  4  \w     97.00 160.00   1.00   35.00    --  107.09 125.00 -60.00   63
  5  \w     32.00 134.00   1.00   35.00    --  107.09 -30.00-180.00  102
  6  \w     39.00 112.00   1.00   35.00    --  107.09-125.00-180.00   73
  7  \w     81.00 172.00   1.00   35.00    --  107.09  45.00   0.00   91
  8  \w    100.00 175.00   1.00   35.00    --  107.09  45.00 120.00   75
  9  \w     25.00 100.00   1.00   35.00    --  107.09 -94.00  30.00   75
 10  \w     98.00 123.00   1.00   35.00    --  107.09 125.00-150.00   25
 11  \w    140.00 167.00   1.00   35.00    --  107.09 125.00-150.00   27
 12  \w     46.00 106.00   1.00   35.00    --  107.09 -94.00 -60.00   60
 13  \w     41.00 106.00   1.00   35.00    --  107.09 -94.00-150.00   65
 14  \w     31.00 124.00   1.00   35.00    --  107.09 -30.00 -30.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3523
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.221
_diffrn_reflns_theta_min         4.073
_exptl_absorpt_coefficient_mu    3.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.230
_exptl_crystal_description       plank
_exptl_crystal_F_000             396
_exptl_crystal_preparation
'Prepared in-situ under crystallization conditions'
_exptl_crystal_recrystallization_method
'Grown from a biphasic mixture of an aqueous solution containing the metal salt and a perfluorocarbon phase containing the acac ligand'
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.977
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1454P)^2^+0.1056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2017
_reflns_number_total             2188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00691j2.cif
_cod_data_source_block           oepg_zn12
_cod_original_cell_volume        607.43(12)
_cod_database_code               7709866
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O3(H3A,H3B)
;
_shelx_res_checksum              63084
_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
;