Syntheses and electronic structures of mu-nitrido bridged pyridine, diimine iridium complexes
Friedrich Angersbach-Bludau; Christopher Schulz; Julia Schoffel; Peter Burger; Chem.Commun. 50 (2014) 8735–; doi:10.1039/C4cc03624G

data_7115372
_publ_section_title
;
 Syntheses and electronic structures of mu-nitrido bridged pyridine,
 diimine iridium complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8735
_journal_paper_doi               10.1039/C4cc03624G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C50 H54 Ir2 N7, C4 H8 O1, Na1'
_chemical_formula_sum            'C54 H62 Ir2 N7 Na O'
_chemical_formula_weight         1232.50
_chemical_melting_point          ?
_chemical_name_common            '[Ir(C25H27N3)N3Ir(C25H27N3)]CF3SO3*C7H8'
_chemical_name_systematic
; 
 [Ir(Me4N3)NIr(Me4N3)]OTf 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.3510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.69290(10)
_cell_length_b                   26.4273(2)
_cell_length_c                   16.81080(10)
_cell_measurement_reflns_used    11211
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.88
_cell_volume                     4736.78(6)
_computing_cell_refinement       'SAINT (Bruker AXS, 2008)'
_computing_data_collection       'SMART (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997-2005 Glasgow)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62794
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'incoatec microfocus'
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    5.670
_exptl_absorpt_correction_T_max  0.8483
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 1998)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         11211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+6.9336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0489
_reflns_number_gt                9875
_reflns_number_total             11211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc03624g2.cif
_cod_data_source_block           2211
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C54 H62 Ir2 N7 Na1 O1'
_cod_database_code               7115372
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3A(0.041) H3B(0.041) H3C(0.041) H4(0.033) H5(0.036) H6(0.034)
 H8A(0.041) H8B(0.041) H8C(0.041) H10A(0.044) H10B(0.044) H10C(0.044)
 H12(0.027) H13(0.027) H14(0.026) H17A(0.035) H17B(0.035) H17C(0.035)
 H20A(0.037) H20B(0.037) H20C(0.037) H21(0.034) H22(0.039) H23(0.036)
 H25A(0.045) H25B(0.045) H25C(0.045) H28A(0.049) H28B(0.049) H28C(0.049)
 H29(0.036) H30(0.04) H31(0.038) H33A(0.05) H33B(0.05) H33C(0.05) H35A(0.045)
 H35B(0.045) H35C(0.045) H37(0.029) H38(0.032) H39(0.028) H42A(0.04) H42B(0.04)
 H42C(0.04) H45A(0.035) H45B(0.035) H45C(0.035) H46(0.033) H47(0.039)
 H48(0.038) H50A(0.05) H50B(0.05) H50C(0.05) H51A(0.044) H51B(0.044)
 H52A(0.052) H52B(0.052) H53A(0.05) H53B(0.05) H54A(0.04) H54B(0.04)
 Fixed X: H3A(0.4644) H3B(0.5594) H3C(0.4783) H4(0.7581) H5(0.9103) H6(0.8656)
 H8A(0.6125) H8B(0.6046) H8C(0.7325) H10A(0.4649) H10B(0.3221) H10C(0.4227)
 H12(0.1679) H13(0.0154) H14(0.0429) H17A(0.1604) H17B(0.2279) H17C(0.102)
 H20A(0.5508) H20B(0.4336) H20C(0.5655) H21(0.5813) H22(0.5355) H23(0.4197)
 H25A(0.3116) H25B(0.2258) H25C(0.345) H28A(0.2367) H28B(0.3543) H28C(0.3559)
 H29(0.2121) H30(0.2878) H31(0.4994) H33A(0.7072) H33B(0.7103) H33C(0.7396)
 H35A(0.6139) H35B(0.5002) H35C(0.6178) H37(0.8142) H38(1.006) H39(1.0735)
 H42A(1.0443) H42B(1.0993) H42C(1.1198) H45A(0.771) H45B(0.8433) H45C(0.7039)
 H46(0.8007) H47(0.8689) H48(0.9469) H50A(1.0376) H50B(0.9776) H50C(0.8992)
 H51A(0.5563) H51B(0.6458) H52A(0.68) H52B(0.7961) H53A(0.8649) H53B(0.7425)
 H54A(0.7846) H54B(0.6479)
 Fixed Y: H3A(0.4641) H3B(0.4191) H3C(0.4247) H4(0.4635) H5(0.5129) H6(0.5588)
 H8A(0.5955) H8B(0.5464) H8C(0.5751) H10A(0.564) H10B(0.5756) H10C(0.6019)
 H12(0.5782) H13(0.558) H14(0.4897) H17A(0.3724) H17B(0.4118) H17C(0.4263)
 H20A(0.4527) H20B(0.4555) H20C(0.4418) H21(0.3552) H22(0.2712) H23(0.2472)
 H25A(0.2659) H25B(0.3133) H25C(0.3174) H28A(0.3392) H28B(0.363) H28C(0.3527)
 H29(0.2547) H30(0.1748) H31(0.1585) H33A(0.1843) H33B(0.221) H33C(0.2416)
 H35A(0.2584) H35B(0.2959) H35C(0.3089) H37(0.3449) H38(0.3835) H39(0.4094)
 H42A(0.4525) H42B(0.3982) H42C(0.4254) H45A(0.4938) H45B(0.4836) H45C(0.4657)
 H46(0.4362) H47(0.3601) H48(0.2997) H50A(0.3079) H50B(0.2662) H50C(0.2902)
 H51A(0.2142) H51B(0.2444) H52A(0.149) H52B(0.1846) H53A(0.1685) H53B(0.1372)
 H54A(0.2261) H54B(0.2038)
 Fixed Z: H3A(0.4564) H3B(0.4691) H3C(0.3879) H4(0.4883) H5(0.4377) H6(0.3221)
 H8A(0.2394) H8B(0.1871) H8C(0.202) H10A(0.3848) H10B(0.3654) H10C(0.3163)
 H12(0.2511) H13(0.1509) H14(0.0676) H17A(0.0054) H17B(-0.0464) H17C(-0.01)
 H20A(0.0235) H20B(-0.0382) H20C(-0.067) H21(-0.1008) H22(-0.082) H23(0.0216)
 H25A(0.1378) H25B(0.1206) H25C(0.1806) H28A(0.353) H28B(0.3171) H28C(0.409)
 H29(0.3139) H30(0.2951) H31(0.3194) H33A(0.3514) H33B(0.4247) H33C(0.3407)
 H35A(0.5208) H35B(0.5121) H35C(0.5699) H37(0.583) H38(0.5761) H39(0.4545)
 H42A(0.2564) H42B(0.2451) H42C(0.3278) H45A(0.1033) H45B(0.1864) H45C(0.1703)
 H46(-0.0007) H47(-0.0465) H48(0.0421) H50A(0.2302) H50B(0.1728) H50C(0.2383)
 H51A(0.1504) H51B(0.2125) H52A(0.1926) H52B(0.2148) H53A(0.0957) H53B(0.0707)
 H54A(0.0089) H54B(0.0101)
;