Coupling of Aromatic Aldehydes with CO2Me-Substituted TpMe2Ir(III) Metallacyclopentadienes
Roa, Arián E.; Salazar, Verónica; López-Serrano, Joaqu\?ín; Oñate, Enrique; Alvarado-Rodr\?íguez, José G.; Paneque, Margarita; Poveda, Manuel L.; Organometallics 31 (2012) 3185–; doi:10.1021/om3000554

data_4078046
_publ_section_title
;
 Coupling of Aromatic Aldehydes with CO2Me-Substituted TpMe2Ir(III)
 Metallacyclopentadienes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              3185
_journal_paper_doi               10.1021/om3000554
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C44 H55 B Cl4 Ir N7 O13'
_chemical_formula_weight         1234.76
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.087(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.507(3)
_cell_length_b                   20.843(4)
_cell_length_c                   19.049(4)
_cell_measurement_reflns_used    1287
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16.59
_cell_measurement_theta_min      2.24
_cell_volume                     5223.5(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32001
_diffrn_reflns_theta_full        25.15
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  0.3500
_exptl_absorpt_correction_T_min  0.2774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 (Bruker,2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         9319
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                6916
_reflns_number_total             9319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3000554_si_002.cif
_cod_data_source_block           6c_dmo_19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5223.2(17)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078046