Cyclometalated Ir(iii) complexes of deprotonated N-methylbipyridinium ligands: effects of quaternised N centre position on luminescence.
Coe, Benjamin J.; Helliwell, Madeleine; Raftery, James; Sánchez, Sergio; Peers, Martyn K.; Scrutton, Nigel S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20392–20405; doi:10.1039/c5dt03753k

data_7036907
_publ_section_title
;
 Cyclometalated Ir(iii) complexes of deprotonated N-methylbipyridinium
 ligands: effects of quaternised N centre position on luminescence.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20392
_journal_page_last               20405
_journal_paper_doi               10.1039/c5dt03753k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C34 H26 F6 Ir N6, 2(C4 H8 O2), 3(F6 P)'
_chemical_formula_sum            'C42 H42 F24 Ir N6 O4 P3'
_chemical_formula_weight         1435.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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
_audit_creation_date             2015-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-09-25 deposited with the CCDC.
2015-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.4620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2871(4)
_cell_length_b                   19.2131(5)
_cell_length_c                   37.1997(9)
_cell_measurement_temperature    100(2)
_cell_volume                     10192.7(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_laue_measured_fraction_full 0.984
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            34713
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.592
_diffrn_reflns_theta_max         66.592
_diffrn_reflns_theta_min         3.860
_exptl_absorpt_coefficient_mu    7.225
_exptl_absorpt_correction_T_max  0.5966
_exptl_absorpt_correction_T_min  0.333706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       block
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         8853
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+96.7014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8413
_reflns_number_total             8853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03753k2.cif
_cod_data_source_block           s3690ma
_cod_depositor_comments
'Adding full bibliography for 7036902--7036907.cif.'
_cod_database_code               7036907
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.341
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C4AA
 1.43 with sigma of 0.02
 O1-C5
 1.43 with sigma of 0.02
3. Rigid bond restraints
 C5, O1, C4AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C5, O1, C4AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C4AA(H4AA,
 H4AB), C5(H5A,H5B), C39(H39A,H39B), C40(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1AA(H1AA), C3AA(H3AA), C7(H7), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C31(H31), C32(H32), C33(H33)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C34(H34A,H34B,H34C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'