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_7017931
_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, 2(C3 H7 N O)'
_chemical_formula_sum            'C42 H60 Cl4 Ir2 N6 O4'
_chemical_formula_weight         1239.208
_chemical_name_systematic
;
[my2-(1,4-bis(4-nitrosophenyl)piperazin-N,N)bis
(dichlorido-(eta5-pentamethyl-cyclopentadienyl)-iridium(III))]'
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             05-Jun-08
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.620(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.4121(6)
_cell_length_b                   8.7721(4)
_cell_length_c                   16.3489(7)
_cell_measurement_reflns_used    29561
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      3.134
_cell_volume                     2270.13(17)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27313
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         3.22
_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    6.139
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.636
_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            red
_exptl_crystal_density_diffrn    1.81292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method
'slow isothermic diffusion of n-pentane into a nearly saturated solution in DMF'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0162P)^2^+3.0451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0542
_reflns_number_gt                3387
_reflns_number_total             4174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11696g.txt
_cod_data_source_block           7a_CCDC-000000
_cod_original_cell_volume        2270.13(16)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017931
_kl_diffrn_measurement_scan_angle phi/omega-scan
_kl_diffrn_measurement_scan_step_degree 2.0
_kl_diffrn_measurement_scan_time_per_degree 20
_kl_diffrn_measurement_detector_distance 30