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_7036906
_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         'C32 H28 Ir N6, 3(F6 P), C4 H10 O, C2 H3 N'
_chemical_formula_sum            'C38 H41 F18 Ir N7 O P3'
_chemical_formula_weight         1238.89
_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
_audit_creation_date             2015-09-24
_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                 101.7760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2122(7)
_cell_length_b                   21.6961(12)
_cell_length_c                   17.2606(9)
_cell_measurement_reflns_used    6573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.124
_cell_measurement_theta_min      2.231
_cell_volume                     4477.1(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25575
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.358
_diffrn_reflns_theta_min         1.877
_exptl_absorpt_coefficient_mu    3.207
_exptl_absorpt_correction_T_max  0.5664
_exptl_absorpt_correction_T_min  0.453936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         9101
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.405
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+9.1204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7424
_reflns_number_total             9101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03753k2.cif
_cod_data_source_block           s3652a
_cod_depositor_comments
'Adding full bibliography for 7036902--7036907.cif.'
_cod_database_code               7036906
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.360
_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. Rigid bond restraints
 F1, F2, F3, F4, F5, F6, F7, F8, F9, F10, F11, F12, F13, F14, F15, F16, F17, F18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17
\\sim F18: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.0001
4. Same fragment restrains
{P2, F7, F8, F9, F10, F11, F12} sigma for 1-2: 0.02, 1-3: 0.04
{P3, F13, F14, F15, F16, F17, F18} sigma for 1-2: 0.02, 1-3: 0.04
as
{P1, F1, F2, F3, F4, F5, F6}
5.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,
 H4SC), C5S(H5SA,H5SB,H5SC)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'