Transition metal-free, visible-light mediated synthesis of 1,10-phenanthroline derived ligand systems
Edwards, Alyn C.; Geist, Andreas; Müllich, Udo; Sharrad, Clint A.; Pritchard, Robin G.; Whitehead, Roger C.; Harwood, Laurence M.; Chemical Communications 53 (2017) 8160–8163; doi:10.1039/C7CC03903D

data_1546413
_publ_section_title
;
 Transition metal-free, visible-light mediated synthesis of
 1,10-phenanthroline derived ligand systems
;
_journal_issue                   58
_journal_name_full               'Chemical Communications'
_journal_page_first              8160
_journal_page_last               8163
_journal_paper_doi               10.1039/C7CC03903D
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C37 H48 N8 O2'
_chemical_formula_weight         636.83
_chemical_name_systematic        4,7-Me-CyMe4-BTPhen
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.832(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   8.6647(5)
_cell_length_c                   23.1992(12)
_cell_measurement_reflns_used    2574
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.15
_cell_measurement_theta_min      3.02
_cell_volume                     3361.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_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  0.0604
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22281
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.257
_diffrn_reflns_theta_min         3.022
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.830644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0909P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4903
_reflns_number_total             6587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03903d2.cif
_cod_data_source_block           s4608ma
_cod_database_code               1546413
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              8985