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_4038975
_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         'C34 H28 Br N4 O5 Re'
_chemical_formula_sum            'C34 H28 Br N4 O5 Re'
_chemical_formula_weight         838.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                111.784(8)
_cell_angle_beta                 110.740(8)
_cell_angle_gamma                97.685(7)
_cell_formula_units_Z            2
_cell_length_a                   11.1587(8)
_cell_length_b                   13.0479(10)
_cell_length_c                   13.1431(10)
_cell_measurement_reflns_used    9075
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     1582.4(3)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_data_reduction
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_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 0.989
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19957
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    5.150
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.3369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       column
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.087
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0511P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6334
_reflns_number_total             7218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2013ncs0317.cif
_cod_data_source_block           2013ncs0317
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__computing_structure_solution' was replaced with
'_computing_structure_solution'.

Automatic conversion script
Id: cif_correct_tags 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        1582.4(2)
_cod_database_code               4038975
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.337
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C23(H23), C24(H24), C26(H26), C27(H27)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              51550
_shelx_hkl_checksum              54460
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'