Zinc(II)-Mediated Carbene Insertion into C-H Bonds in Alkanes.
Kulkarni, Naveen V.; Dash, Chandrakanta; Jayaratna, Naleen B.; Ridlen, Shawn G.; Karbalaei Khani, Sarah; Das, Animesh; Kou, Xiaodi; Yousufuddin, Muhammed; Cundari, Thomas R.; Dias, H. V. Rasika; Inorganic chemistry 54 (2015) 11043–11045; doi:10.1021/acs.inorgchem.5b02134

data_4344452
_publ_section_title
;
 Zinc(II)-Mediated Carbene Insertion into C-H Bonds in Alkanes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11043
_journal_page_last               11045
_journal_paper_doi               10.1021/acs.inorgchem.5b02134
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C19 H10 B Cl F18 N8 O4 Zn, C H2 Cl2'
_chemical_formula_sum            'C20 H12 B Cl3 F18 N8 O4 Zn'
_chemical_formula_weight         952.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.5690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9470(12)
_cell_length_b                   14.3993(13)
_cell_length_c                   18.3661(17)
_cell_measurement_reflns_used    8135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.24
_cell_volume                     3394.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         1.803
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;The unit cell contains 4 methylene chloride molecules which have been 
treated as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON 
;
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.6442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6762
_reflns_number_total             8451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02134_si_002.cif
_cod_data_source_block           dias760m_a
_cod_depositor_comments          'Adding full bibliography for 4344452.cif.'
_cod_database_code               4344452
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.835
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              6612
_shelx_hkl_checksum              99398
_shelx_fab_checksum              46947