Unraveling the Competition of Two C‒H and Two M‒C Bonds in Guiding the Mechanism of Rhodium(III)-Catalyzed C‒H Activation‒Annulation
Thenarukandiyil, Ranjeesh; Gupta, Suraj K.; Choudhury, Joyanta; ACS Catalysis 6 (2016) 5132–; doi:10.1021/acscatal.6b01486

data_4513905
_publ_section_title
;
 Unraveling the Competition of Two C--H and Two M--C Bonds in Guiding the
 Mechanism of Rhodium(III)-Catalyzed C--H Activation--Annulation
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              5132
_journal_paper_doi               10.1021/acscatal.6b01486
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C26 H30 I Ir N2 O4'
_chemical_formula_weight         753.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.437(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.646(3)
_cell_length_b                   17.272(5)
_cell_length_c                   14.564(5)
_cell_measurement_reflns_used    3980
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.18
_cell_volume                     2624.8(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31885
_diffrn_reflns_theta_full        23.82
_diffrn_reflns_theta_max         23.82
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    6.296
_exptl_absorpt_correction_T_max  0.6328
_exptl_absorpt_correction_T_min  0.3970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.873
_refine_diff_density_rms
'0.261 ===========================================END'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+34.5728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                3278
_reflns_number_total             3980
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cs6b01486_si_002.cif
_cod_data_source_block           6_Ir
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4513904--4513906.cif.
;
_cod_original_cell_volume        2624.8(13)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               4513905