Diverse reactivity of carbenes and silylenes towards fluoropyridines.
Kundu, Gargi; Ajithkumar, V. S.; Bisai, Milan Kumar; Tothadi, Srinu; Das, Tamal; Vanka, Kumar; Sen, Sakya S.; Chemical communications (Cambridge, England) 57 (2021) 4428–4431; doi:10.1039/d1cc01401c

data_7128072
_publ_section_title
;
 Diverse reactivity of carbenes and silylenes towards fluoropyridines.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4428
_journal_page_last               4431
_journal_paper_doi               10.1039/d1cc01401c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'B C18 F16, C27 H39 N2, 2(C6 H6)'
_chemical_formula_sum            'C57 H51 B F16 N2'
_chemical_formula_weight         1078.80
_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   geom
_audit_creation_date             2021-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-12 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                83.095(18)
_cell_angle_beta                 83.19(2)
_cell_angle_gamma                70.263(12)
_cell_formula_units_Z            2
_cell_length_a                   10.350(2)
_cell_length_b                   11.9292(18)
_cell_length_c                   22.376(12)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.22
_cell_volume                     2572.5(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36558
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.587
_diffrn_reflns_theta_min         1.820
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1618 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.9184.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         10653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+3.6855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8719
_reflns_number_total             10653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01401c2.cif
_cod_data_source_block           gk241019_0m-auto
_cod_depositor_comments
'Adding full bibliography for 7128070--7128074.cif.'
_cod_database_code               7128072
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.974
_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 Ternary CH refined with riding coordinates:
 C30(H30), C35(H35), C40(H40), C49(H49)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C0AA(H0AA), C3(H3), C4(H4), C5(H5), C6(H6), C26(H26),
 C27(H27), C28(H28), C37(H37), C38(H38), C45(H45), C46(H46), C47(H47), C54(H54),
  C55(H55), C56(H56), C57(H57)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C)
;
_shelx_res_checksum              45274
_shelx_hkl_checksum              51519
_olex2_submission_special_instructions 'No special instructions were received'