Synthesis, structure, and excited state kinetics of heteroleptic Cu(i) complexes with a new sterically demanding phenanthroline ligand
Kohler, Lars; Hadt, Ryan G.; Hayes, Dugan; Chen, Lin X.; Mulfort, Karen L.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02476B

data_7044317
_publ_section_title
;
 Synthesis, structure, and excited state kinetics of heteroleptic Cu(i)
 complexes with a new sterically demanding phenanthroline ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02476B
_journal_year                    2017
_chemical_formula_sum            'C60 H74 Cu F6 N4 O P'
_chemical_formula_weight         1075.74
_chemical_name_systematic
'(2,9-bis(2,4,6-triisopropylphenyl)-1,10-phenanthroline)-(2,9-dimethyl-1,10-phenanthroline)-copper hexafluorophosphate diethyl ether solvate'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-30 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.164(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.851(9)
_cell_length_b                   19.517(7)
_cell_length_c                   25.628(9)
_cell_measurement_reflns_used    113809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.835
_cell_measurement_theta_min      1.043
_cell_volume                     11430(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 3.3'
_computing_publication_material  'Mercury 3.3'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '0.5 Deg w/ exposures'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0862
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            113809
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.835
_diffrn_reflns_theta_min         1.043
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       'prismatic rod'
_exptl_crystal_F_000             4544
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.207
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1348
_refine_ls_number_reflns         25454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0821
_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^)+66.2137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18718
_reflns_number_total             25454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02476b2.cif
_cod_data_source_block           'data_0m'
_cod_depositor_comments
;

2018-02-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C120 H148 Cu2 F12 N8 O2 P2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2151.48
_cod_database_code               7044317
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              20531