Synthesis, structure, and reactions of a nitroxyl complex of iridium(iii), cis,trans-IrHCl2(NHO)(PPh3)2
Melenkivitz, Rory; Hillhouse, Gregory L.; Chemical Communications  (2002) 660–; doi:10.1039/b111645b

data_7114305
_publ_section_title
;
 Synthesis, structure, and reactions of a nitroxyl complex of
 iridium(iii), cis,trans-IrHCl2(NH&#xE001;O)(PPh3)2
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              660
_journal_paper_doi               10.1039/b111645b
_journal_year                    2002
_chemical_formula_sum            'C51 H55 Cl2 Ir N O4 P2'
_chemical_formula_weight         1071.00
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.508(2)
_cell_angle_beta                 84.582(2)
_cell_angle_gamma                64.976(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9751(11)
_cell_length_b                   11.1216(12)
_cell_length_c                   23.281(3)
_cell_measurement_temperature    100
_cell_volume                     2318.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.819
_diffrn_measured_fraction_theta_max 0.819
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.1005
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13810
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_correction_T_min  0.3693
_exptl_absorpt_correction_type   'semi-emperical from psi scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1082
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.727
_refine_diff_density_min         -5.453
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9458
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          7.010
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+20.9098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                8375
_reflns_number_total             9458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111645b.txt
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '100 K' was changed to '100' -
the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '100 K' was changed
to '100' - the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2318.2(4)
_cod_database_code               7114305