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_7115370
_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
'C58 H70 Ir2 N7, C24 H20 B, 0.5(C6 H14), C4 H8 O'
_chemical_formula_sum            'C89 H105 B Ir2 N7 O'
_chemical_formula_weight         1684.1047
_chemical_name_common            '[Ir(C29H35N3)NIr(C29H35N3)][BC24H20]'
_chemical_name_systematic
; 
[Ir(tBuN3Me4)NIr(tBuN3Me4)][BPh4] 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.97
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8882(3)
_cell_length_b                   23.2366(5)
_cell_length_c                   15.1330(3)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.997
_cell_measurement_theta_min      4.470
_cell_volume                     4157.69(16)
_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, 1997-2008 Glasgow)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       omega-scan
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            105248
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.245
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1710
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.235
_refine_diff_density_min         -1.746
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         29402
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+7.5677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                24963
_reflns_number_total             29402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc03624g2.cif
_cod_data_source_block           fa159hv
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        4157.66(16)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7115370