Synthesis, Structure, and Reactivity of Aliphatic Primary Nitrosamines Stabilized by Coordination to [IrCl5]2−
Di Salvo, Florencia; Estrin, Darío A.; Leitus, Gregory; Doctorovich, Fabio; Organometallics 27 (2008) 1985–; doi:10.1021/om700985h

data_4070750
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Aliphatic Primary Nitrosamines
 Stabilized by Coordination to [IrCl5]2&#x2212;
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1985
_journal_paper_doi               10.1021/om700985h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C55 H48 Cl5 Ir N2 O4 P2'
_chemical_formula_weight         1232.34
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.69(3)
_cell_angle_beta                 65.47(3)
_cell_angle_gamma                66.00(3)
_cell_formula_units_Z            2
_cell_length_a                   14.039(3)
_cell_length_b                   14.109(3)
_cell_length_c                   16.251(3)
_cell_measurement_reflns_used    11071
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2643.0(14)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7588
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    2.886
_exptl_absorpt_correction_T_max  0.7612
_exptl_absorpt_correction_T_min  0.5960
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.638
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         7588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0129P)^2^+27.4309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                6738
_reflns_number_total             7588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700985h-file002.cif
_cod_data_source_block           m541a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        2643.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4070750