Zinc-Mediated Carbene Insertion to C-Cl Bonds of Chloromethanes and Isolable Zinc(II) Isocyanide Adducts.
Kulkarni, Naveen V.; Das, Animesh; Jayaratna, Naleen B.; Yousufuddin, Muhammed; Dias, H. V. Rasika; Inorganic chemistry 54 (2015) 5151–5153; doi:10.1021/acs.inorgchem.5b00929

data_4346199
_publ_section_title
;
 Zinc-Mediated Carbene Insertion to C-Cl Bonds of Chloromethanes and
 Isolable Zinc(II) Isocyanide Adducts.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5151
_journal_page_last               5153
_journal_paper_doi               10.1021/acs.inorgchem.5b00929
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C25 H22 B F18 N8 Zn, C32 H12 B F24'
_chemical_formula_sum            'C57 H34 B2 F42 N8 Zn'
_chemical_formula_weight         1715.91
_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     direct
_audit_creation_date             2015-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.6780(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9929(15)
_cell_length_b                   17.0158(14)
_cell_length_c                   23.900(2)
_cell_measurement_reflns_used    9216
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      37.33
_cell_measurement_theta_min      2.95
_cell_volume                     6890.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62349
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.750
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8182
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0916 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.8182.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       clear
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.222
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         12162
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1435
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1432P)^2^+5.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6799
_reflns_number_total             12162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00929_si_002.cif
_cod_data_source_block           rad123_0m_a
_cod_database_code               4346199
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.871
_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. Uiso/Uaniso restraints and constraints
Uanis(F23) \\sim Ueq, Uanis(F40) \\sim Ueq, Uanis(F41) \\sim Ueq, Uanis(F42)
\\sim Ueq, Uanis(F40A) \\sim Ueq, Uanis(F41A) \\sim Ueq, Uanis(F42A) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F31) \\sim Ueq, Uanis(F38) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(F28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(F40A)=Sof(F41A)=Sof(F42A)=1-FVAR(1)
 Sof(F40)=Sof(F41)=Sof(F42)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12), C27(H27), C29(H29), C31(H31), C35(H35), C37(H37),
 C39(H39), C43(H43), C45(H45), C47(H47), C51(H51), C53(H53), C55(H55)
4.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'