Protonation Reactions of Dinuclear Pyrazolato Iridium(I) Complexes
Cristina Tejel; Miguel A. Ciriano; Marta Millaruelo; José A. López; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 42 (2003) 4750–4758; doi:10.1021/ic034225x

data_4313914
_publ_contact_author_address
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@posta.unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Fernando J. Lahoz'
_publ_contact_author_phone       '+34 976 761147'
_publ_section_title
;
 Protonation Reactions of Dinuclear Pyrazolato Iridium(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4750
_journal_page_last               4758
_journal_paper_doi               10.1021/ic034225x
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C44 H38 Cl2 Ir2 N4 O8 P2'
_chemical_formula_sum            'C44 H38 Cl2 Ir2 N4 O8 P2'
_chemical_formula_weight         1268.02
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.9120(10)
_cell_angle_beta                 88.7760(10)
_cell_angle_gamma                84.3340(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5095(6)
_cell_length_b                   13.8588(9)
_cell_length_c                   17.6696(12)
_cell_measurement_reflns_used    5141
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.15
_cell_volume                     2189.7(2)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26900
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    6.324
_exptl_absorpt_correction_T_max  0.7427
_exptl_absorpt_correction_T_min  0.2445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.563
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         10287
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0207P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                8361
_reflns_number_total             10287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034225xsi20030228_071656_2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313914