1,4-Bis(4-nitrosophenyl)piperazine: novel bridging ligand in dinuclear complexes of rhodium(iii) and iridium(iii).
Wirth, Stefan; Barth, Florian; Lorenz, Ingo-Peter; Dalton transactions (Cambridge, England : 2003) 41 (2012) 2176–2186; doi:10.1039/c1dt11696g

data_7017932
_publ_section_title
;
 1,4-Bis(4-nitrosophenyl)piperazine: novel bridging ligand in dinuclear
 complexes of rhodium(iii) and iridium(iii).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2176
_journal_page_last               2186
_journal_paper_doi               10.1039/c1dt11696g
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C36 H46 Cl4 Ir2 N4 O2, 5(C H Cl3)'
_chemical_formula_sum            'C41 H51 Cl19 Ir2 N4 O2'
_chemical_formula_weight         1689.905
_chemical_name_systematic
;
[my2-(1,4-bis(4-nitrosophenyl)piperazin-N,N)bis
(dichlorido-(eta5-pentamethyl-cyclopentadienyl)-iridium(III))]
;
_chemical_properties_physical    moisture-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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_date             23-Jan-08
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.1180(10)
_cell_angle_beta                 95.346(2)
_cell_angle_gamma                97.882(2)
_cell_formula_units_Z            4
_cell_length_a                   15.6660(4)
_cell_length_b                   17.5276(5)
_cell_length_c                   23.5115(6)
_cell_measurement_reflns_used    163761
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.134
_cell_volume                     6227.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
;
Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst. 1997, 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images'
_diffrn_radiation_collimation    0.25
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70571
_diffrn_reflns_theta_full        23.04
_diffrn_reflns_theta_max         23.04
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           55.00
_diffrn_source_power             3.025
_diffrn_source_voltage           55.00
_exptl_absorpt_coefficient_mu    5.121
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. SADABS. Version 2. Multi-Scan Absorption Correction.
University of Goettingen, Germany, 2001
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.80251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3272
_exptl_crystal_recrystallization_method
;
slow isothermic diffusion of n-pentane into
a nearly saturated solution in C
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The unit cell contains 2 additional molecules (one per asymmetric unit)
of CHCl3 which have been treated as diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.596
_refine_diff_density_min         -1.797
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         17274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0647P)^2^+25.6477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                13475
_reflns_number_total             17274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11696g.txt
_cod_data_source_block           7a`_CCDC-000000
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               7017932
_kl_diffrn_measurement_scan_angle omega-scan
_kl_diffrn_measurement_scan_step_degree 1.0
_kl_diffrn_measurement_scan_time_per_degree 35
_kl_diffrn_measurement_detector_distance 30