N-Metallacycles from [Cp*MX2]2and Alkynylpyridines: Synthesis, Reaction Pathway, and Aromaticity
Teo, Jing Wei; Sridevi, Venugopal Shanmugham; Leong, Weng Kee; Organometallics 33 (2014) 1174–; doi:10.1021/om401154c

data_4082693
_publ_section_title
;
 N-Metallacycles from [Cp*MX2]2and Alkynylpyridines: Synthesis, Reaction
 Pathway, and Aromaticity
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1174
_journal_paper_doi               10.1021/om401154c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C17 H20 Cl2 Ir N'
_chemical_formula_weight         501.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.71(3)
_cell_angle_beta                 74.99(3)
_cell_angle_gamma                64.67(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1568(16)
_cell_length_b                   8.2765(17)
_cell_length_c                   14.305(3)
_cell_measurement_reflns_used    4312
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.89
_cell_measurement_theta_min      2.70
_cell_volume                     837.3(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23565
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    8.284
_exptl_absorpt_correction_T_max  0.6363
_exptl_absorpt_correction_T_min  0.1449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3420
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+1.6104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0543
_reflns_number_gt                3305
_reflns_number_total             3420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401154c_si_002.cif
_cod_data_source_block           sd34one
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        837.4(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082693