Site-selective metallation of dicarbene precursors.
Bente, Stefanie; Kampert, Florian; Tan, Tristan T. Y.; Hahn, F. Ekkehardt; Chemical communications (Cambridge, England) 54 (2018) 12887–12890; doi:10.1039/c8cc08440h

data_7122495
_publ_section_title
;
 Site-selective metallation of dicarbene precursors.
;
_journal_issue                   91
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12887
_journal_page_last               12890
_journal_paper_doi               10.1039/c8cc08440h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C20 H20 Cl I N4'
_chemical_formula_weight         478.75
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-08-08 deposited with the CCDC.
2018-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0786(2)
_cell_length_b                   11.8861(2)
_cell_length_c                   11.9437(2)
_cell_measurement_reflns_used    6065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7985
_cell_measurement_theta_min      3.5705
_cell_volume                     1984.73(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22242
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         31.006
_diffrn_reflns_theta_min         3.381
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Multi-scan correction included in APEX3 package (Bruker AXS, 2014)
 22803 Corrected reflections used
 Estimated minimum and maximum transmission:  0.6930  0.7960
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.1550
 Lambda/2 correction factor = 0.00150
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         6250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5105
_reflns_number_total             6250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08440h2.cif
_cod_data_source_block           sbs2
_cod_depositor_comments
'Adding full bibliography for 7122494--7122497.cif.'
_cod_database_code               7122495
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.547
_shelx_estimated_absorpt_t_max   0.859
_shelx_res_checksum              45060
_shelx_hkl_checksum              36204