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_7017934
_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 I4 Ir2 N4 O2, C H2 Cl2'
_chemical_formula_sum            'C37 H48 Cl2 I4 Ir2 N4 O2'
_chemical_formula_weight         1543.760
_chemical_name_systematic
;
[my2-(1,4-bis(4-nitrosophenyl)piperazin-N,N)bis
((eta5-pentamethyl-cyclopentadienyl)-diiodido-iridium(III))]
;
_chemical_properties_physical    moisture-sensitive
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             20-Oct-09
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.264(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.9917(12)
_cell_length_b                   11.4311(8)
_cell_length_c                   14.4137(8)
_cell_measurement_reflns_used    7643
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      3.134
_cell_volume                     4523.2(5)
_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; 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  0.0969
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28982
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         3.35
_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    8.761
_exptl_absorpt_correction_T_max  0.9170
_exptl_absorpt_correction_T_min  0.7026
_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            black
_exptl_crystal_density_diffrn    2.2670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2856
_exptl_crystal_recrystallization_method
'slow isothermic diffusion of n-pentane into a nearly saturated solution in DCM'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains 4 additional molecules (1 per asymmetric unit)
of CH2Cl2 which have been treated as diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+3.0807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                3095
_reflns_number_total             4118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11696g.txt
_cod_data_source_block           7c_CCDC-000000
_cod_original_cell_volume        4523.2(4)
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7017934
_kl_diffrn_measurement_scan_angle phi/omega-scan
_kl_diffrn_measurement_scan_step_degree 2.0
_kl_diffrn_measurement_scan_time_per_degree 60
_kl_diffrn_measurement_detector_distance 30