[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_7237411
_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)(Et-S-Bipy)][PF6]. 1.5(Et2O)'
_chemical_formula_sum            'C57 H59 Cu F6 N2 O2.5 P3 S'
_chemical_formula_weight         1114.63
_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             2016-05-24
_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                95.111(3)
_cell_angle_beta                 93.760(3)
_cell_angle_gamma                107.807(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9194(5)
_cell_length_b                   15.3624(8)
_cell_length_c                   16.8151(9)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    123
_cell_measurement_theta_max      69
_cell_measurement_theta_min      3
_cell_volume                     2662.0(2)
_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 0.975
_diffrn_measured_fraction_theta_max 0.941
_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  0.039
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31869
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         70.092
_diffrn_reflns_theta_min         3.799
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1158
_exptl_crystal_recrystallization_method
; 
DCM / Et2O 
;
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
this equates to 20 e-/formula unit that can be rationalised as
0.5 extra molecule of Et2O per formula unit.
ALL the numbers and formulae have been modified to keep this result in account.
;
_refine_diff_density_max         1.43
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9434
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.0004923
_refine_ls_shift/su_mean         0.0000173
_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: 
 3.73 5.02 1.41 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1481
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1479
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8534
_reflns_number_total             9530
_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   0.0651
_oxford_refine_ls_scale          0.10030(4)
_oxford_reflns_number_all        9462
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'ALM051_123K_0m in P-1'
_cod_data_source_file            c8tc02882f2.cif
_cod_data_source_block           ALM051_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        'C57 H59 Cu1 F6 N2 O2.50 P3 S1 '
_cod_database_code               7237411