Synthesis and characterisation of homoleptic 2,9-diaryl-1,10-phenanthroline copper(i) complexes: influencing selectivity in photoredox-catalysed atom-transfer radical addition reactions.
Nicholls, Thomas P.; Caporale, Chiara; Massi, Massimiliano; Gardiner, Michael G.; Bissember, Alex C.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7290–7301; doi:10.1039/c8dt04116d

data_7049134
_publ_section_title
;
 Synthesis and characterisation of homoleptic
 2,9-diaryl-1,10-phenanthroline copper(i) complexes: influencing
 selectivity in photoredox-catalysed atom-transfer radical addition
 reactions.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7290
_journal_page_last               7301
_journal_paper_doi               10.1039/c8dt04116d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C52 H28 Cu F12 N4, F6 P, 0.5(C4 H6 N2)'
_chemical_formula_sum            'C54 H31 Cu F18 N5 P'
_chemical_formula_weight         1186.35
_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
_audit_creation_date             2018-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-19 deposited with the CCDC.    2019-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.8790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3534(7)
_cell_length_b                   25.1829(12)
_cell_length_c                   13.9516(7)
_cell_measurement_reflns_used    8442
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      48.23
_cell_measurement_theta_min      3.51
_cell_volume                     4811.5(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker AXS PHOTON-100'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11427
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        48.545
_diffrn_reflns_theta_max         48.545
_diffrn_reflns_theta_min         3.510
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.000
_exptl_absorpt_correction_T_max  0.7496
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0605 before and 0.0529 after correction. The Ratio of minimum to maximum transmission is 0.8977. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         2291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0272P)^2^+16.9821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2018
_reflns_number_total             2291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04116d2.cif
_cod_data_source_block           15tn012_0m
_cod_depositor_comments
'Adding full bibliography for 7049133--7049136.cif.'
_cod_database_code               7049134
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.856
_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. Others
 Sof(F7)=Sof(F8)=Sof(F9)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Fixed Sof: H28A(0.5) H28C(0.5) H28B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17),
 C18(H18), C20(H20), C21(H21), C23(H23), C24(H24)
3.b Idealised Me refined as rotating group:
 C28(H28A,H28C,H28B)
;
_olex2_submission_original_sample_id 15TN012
_olex2_submission_special_instructions 'No special instructions were received'