P-H activation of secondary phosphanes on a parent amido diiridium complex.
Mena, Inmaculada; Casado, Miguel A.; Polo, Víctor; García-Orduña, Pilar; Lahoz, Fernando J.; Oro, Luis A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1609–1619; doi:10.1039/c3dt52911h

data_7028326
_publ_section_title
;
 P-H activation of secondary phosphanes on a parent amido diiridium
 complex.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1609
_journal_page_last               1619
_journal_paper_doi               10.1039/c3dt52911h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C40 H47 Ir2 N P2, C6 D6'
_chemical_formula_sum            'C46 H47 D6 Ir2 N P2'
_chemical_formula_weight         1072.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   21.7209(10)
_cell_length_b                   10.3274(5)
_cell_length_c                   33.4874(16)
_cell_measurement_reflns_used    22992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.235
_cell_volume                     7511.9(6)
_computing_cell_refinement
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_collection       'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_data_reduction
'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material
'XCIF program, SHELXTLv6.12, BrukerAXS; PARST(Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX DUO CCD system'
_diffrn_measurement_method       'narrow \w frames'
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            85822
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.54
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.199
_exptl_absorpt_correction_T_max  0.446
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS 
 within APEX2 package. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;
 There are very large solvent accessible voids in the structure and a zone where
 residual density peaks are observed. The solvent is highly disordered
 and it cannot be modelled even with several restraints. Therefore, 
 SQUEEZE corrections have been applied. 

 The total potential solvent accesible void volume (959 \A3) and the electron
 count (328 e in the unit cell) may agree with the presence of eight C6D6
 molecules. They have been included in the chemical formula, F000 and density. 
 Results of the SQUEEZE calculations are included at the end of this cif file.
;
_refine_diff_density_max         1.674
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         9153
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+62.5186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                8274
_reflns_number_total             9153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52911h.txt
_cod_data_source_block           cmpnd_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/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_sg_symbol_H-M      'P bca'
_cod_database_code               7028326