[Cu(P^P)(N^N)][PF6] compounds with bis(phosphane) and 6-alkoxy, 6-alkylthio, 6-phenyloxy and 6-phenylthio-substituted 2,2′-bipyridine ligands for light-emitting electrochemical cells
Alkan-Zambada, Murat; Keller, Sarah; Martínez-Sarti, Laura; Prescimone, Alessandro; Junquera-Hernández, José M.; Constable, Edwin C.; Bolink, Henk J.; Sessolo, Michele; Ortí, Enrique; Housecroft, Catherine E.; Journal of Materials Chemistry C 6 (2018) 8460–; doi:10.1039/C8TC02882F

data_7237415
_publ_section_title
;
 [Cu(P^P)(N^N)][PF6] compounds with bis(phosphane) and 6-alkoxy,
 6-alkylthio, 6-phenyloxy and 6-phenylthio-substituted
 2,2&#x2032;-bipyridine ligands for light-emitting electrochemical cells
;
_journal_issue                   31
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              8460
_journal_paper_doi               10.1039/C8TC02882F
_journal_volume                  6
_journal_year                    2018
_chemical_compound_source        'Murat Alkan'
_chemical_formula_moiety         '[Cu(Xantphos)(Ph-S-Bipy)][PF6].0.5(DCM)'
_chemical_formula_sum            'C55.5 H45 Cl Cu F6 N2 O P3 S'
_chemical_formula_weight         1093.95
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2016-05-11
_audit_creation_method           CRYSTALS_ver_14.61_build_5809
_audit_update_record
;
2017-07-16 deposited with the CCDC.
2018-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                80.615(3)
_cell_angle_beta                 84.731(3)
_cell_angle_gamma                83.868(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9025(7)
_cell_length_b                   13.2292(9)
_cell_length_c                   17.8354(12)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    123
_cell_measurement_theta_max      70
_cell_measurement_theta_min      3
_cell_volume                     2516.2(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32882
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         70.250
_diffrn_reflns_theta_min         2.518
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.44
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1122
_exptl_crystal_recrystallization_method
; 
DCM / Et2O
;
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
This equates to 20 e-/formula which corresponds to 0.5 DCM per formula unit.
ALL the formulae and numbers have been modifed to keep account for this result.
;
_refine_diff_density_max         0.98
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.0006936
_refine_ls_shift/su_mean         0.0000257
_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: 
 3.09 4.03 1.10 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1258
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1258
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8267
_reflns_number_total             9230
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0525
_oxford_refine_ls_scale          0.11427(3)
_oxford_reflns_number_all        9180
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'ALM043_123K_0m in P-1'
_cod_data_source_file            c8tc02882f2.cif
_cod_data_source_block           ALM043_123K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C55.5 H45 Cu1 F6 N2 O1 P3 S1 Cl1'
_cod_database_code               7237415