Luminescent copper(i) complexes with bisphosphane and halogen-substituted 2,2'-bipyridine ligands.
Keller, Sarah; Prescimone, Alessandro; Bolink, Henk; Sessolo, Michele; Longo, Giulia; Martínez-Sarti, Laura; Junquera-Hernández, José M; Constable, Edwin C.; Ortí, Enrique; Housecroft, Catherine E.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 14263–14276; doi:10.1039/c8dt01338a

data_7046381
_publ_section_title
;
 Luminescent copper(i) complexes with bisphosphane and halogen-substituted
 2,2'-bipyridine ligands.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14263
_journal_page_last               14276
_journal_paper_doi               10.1039/c8dt01338a
_journal_volume                  47
_journal_year                    2018
_chemical_compound_source        'Sarah Keller'
_chemical_formula_moiety         'C46 H35 Br1 Cu1 F6 N2 O1 P3'
_chemical_formula_sum            'C46 H35 Br Cu F6 N2 O P3'
_chemical_formula_weight         982.16
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2017-11-07
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_audit_update_record
;
2017-11-09 deposited with the CCDC.
2018-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.96(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.652(7)
_cell_length_b                   12.7677(9)
_cell_length_c                   18.624(6)
_cell_measurement_reflns_used    3569
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.5980
_cell_measurement_theta_min      1.6380
_cell_volume                     3482(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'form 35 kbar structure)'
_diffrn_ambient_pressure         4200000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.336
_diffrn_measured_fraction_theta_max 0.292
_diffrn_measurement_device       'Newport IS4CCD (4 circle)'
_diffrn_measurement_device_type  'Pilatus 300K'
_diffrn_measurement_method
;
omega rotation with 0.4 degree frames'_diffrn_detector_area_resol_mean
;
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_radiation_monochromator  'double crystal Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19321
_diffrn_reflns_theta_full        17.041
_diffrn_reflns_theta_max         22.722
_diffrn_reflns_theta_min         1.643
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1984
_exptl_crystal_recrystallization_method ' '
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0954
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         4276
_refine_ls_number_restraints     613
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.0006892
_refine_ls_shift/su_mean         0.0000304
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 198. 235. 79.4 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0879
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0879
_reflns_limit_h_max              17
_reflns_limit_h_min              -9
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                2817
_reflns_number_total             4281
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.45
_oxford_diffrn_Wilson_scale      0.80
_oxford_refine_ls_r_factor_ref   0.0939
_oxford_refine_ls_scale          1.233(3)
_oxford_reflns_number_all        4276
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'sk58_05x_ in P2(1)/c'
_cod_data_source_file            c8dt01338a2.cif
_cod_data_source_block           sk58_05
_cod_depositor_comments
'Adding full bibliography for 7046379--7046389.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C46 H35 Br1 Cu1 F6 N2 O1 P3'
_cod_database_code               7046381
_oxdiff_exptl_absorpt_empirical_full_min 0.661
_oxdiff_exptl_absorpt_empirical_full_max 3.756
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;