Synthesis and characterisation of phosphorescent rhenium(I) complexes of hydroxy- and methoxy-substituted imidazo[4,5- f ]-1,10-phenanthroline ligands
Bonello, R. Owen; Pitak, Mateusz B.; Coles, Simon J.; Hallett, Andrew J.; Fallis, Ian A.; Pope, Simon J.A.; Journal of Organometallic Chemistry 841 (2017) 39–47; doi:10.1016/j.jorganchem.2017.04.021

data_4038974
_publ_section_title
;
 Synthesis and characterisation of phosphorescent rhenium(I) complexes of
 hydroxy- and methoxy-substituted imidazo[4,5- f ]-1,10-phenanthroline
 ligands
;
_journal_name_full               'Journal of Organometallic Chemistry'
_journal_page_first              39
_journal_page_last               47
_journal_paper_doi               10.1016/j.jorganchem.2017.04.021
_journal_volume                  841
_journal_year                    2017
_chemical_formula_moiety         'C35 H30 Br N4 O6 Re'
_chemical_formula_sum            'C35 H30 Br N4 O6 Re'
_chemical_formula_weight         868.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 93.380(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.686(5)
_cell_length_b                   12.634(5)
_cell_length_c                   24.0993(10)
_cell_measurement_reflns_used    11052
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.3
_cell_volume                     3552(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61116
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.594
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_correction_T_min  0.8028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6269
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.314
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0742
_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^)+(0.0475P)^2^+19.7470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5733
_reflns_number_total             6269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2012ncs0441.cif
_cod_data_source_block           2012ncs0441
_cod_database_code               4038974
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C30A
 1.54 with sigma of 0.02
 C29-C30B
 1.54 with sigma of 0.02
 C29-C31A
 1.54 with sigma of 0.02
 C29-C32B
 1.54 with sigma of 0.02
 C29-C32A
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C30A, C31A, C32A, C32B, C30B, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30A \\sim C31A \\sim C32A \\sim C32B \\sim C30B \\sim C32B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C31A, C31B, C32A, C32B, C30A, C30B, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C24(H24), C25(H25), C27(H27), C28(H28)
7.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C30A(H30A,H30B,H30C),
 C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C32B(H32D,H32E,H32F), C30B(H30D,
 H30E,H30F), C31B(H31D,H31E,H31F)
;
_shelx_res_checksum              6760
_shelx_hkl_checksum              16223
_shelx_fab_checksum              47402
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'