Synthesis and Characterization of [Ir(AcacBiMs)(COD)] and [cis-Ir(AcacBiMs)2(COE-OH)]
Serrano, Oracio; Nicasio-Collazo, Juan; Morales, Guadalupe; Alvarado-Monzón, J. Carlos; Torres-Huerta, Aarón; Höpfl, Herbert; López, Jorge A.; Esqueda, Ana C.; Organometallics 33 (2014) 2561–; doi:10.1021/om500230k

data_4083174
_publ_section_title
;
 Synthesis and Characterization of [Ir(AcacBiMs)(COD)] and
 [cis-Ir(AcacBiMs)2(COE-OH)]
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2561
_journal_paper_doi               10.1021/om500230k
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C50 H59 Ir O5, C4 H10 O'
_chemical_formula_sum            'C54 H69 Ir O6'
_chemical_formula_weight         1006.29
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1785(13)
_cell_length_b                   17.563(2)
_cell_length_c                   25.343(3)
_cell_measurement_reflns_used    5806
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.08
_cell_measurement_theta_min      2.30
_cell_volume                     4975.5(10)
_computing_cell_refinement       'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1353
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48289
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         8739
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                7598
_reflns_number_total             8739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500230k_si_001.cif
_cod_data_source_block           79herbm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083173--4083174.cif.
;
_cod_original_cell_volume        4975.6(10)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4083174