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_7046384
_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         '[C49 H38 Cl2 Cu1 N2 O1 P2][PF6]+1(CH2Cl2)'
_chemical_formula_sum            'C50 H40 Cl4 Cu F6 N2 O P3'
_chemical_formula_weight         1097.15
_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             2015-11-27
_audit_creation_method           CRYSTALS_ver_14.61_build_5809
_audit_update_record
;
2017-02-28 deposited with the CCDC.
2018-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                113.273(4)
_cell_angle_beta                 100.571(4)
_cell_angle_gamma                90.543(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2546(11)
_cell_length_b                   14.3360(13)
_cell_length_c                   18.0998(16)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    123
_cell_measurement_theta_max      70
_cell_measurement_theta_min      3
_cell_volume                     2626.3(4)
_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 0.985
_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  0.038
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32725
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         70.249
_diffrn_reflns_theta_min         3.367
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.825
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.64
_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             1116.00
_exptl_crystal_recrystallization_method
; 
DCM / Et2O 
;
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
This equates to 92 e/cell that corresponds to 46 e/formula.
This can be rationalised as one molecule of DCM per formula unit
ALL the formulae have been modified to keep account for this result
;
_refine_diff_density_max         1.49
_refine_diff_density_min         -1.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9428
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         9373
_refine_ls_number_restraints     941
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.1077
_refine_ls_shift/su_max          0.0063029
_refine_ls_shift/su_mean         0.0001558
_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: 
 12.6 19.1 8.49 1.90 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2745
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.2745
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                9049
_reflns_number_total             9421
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.47
_oxford_diffrn_Wilson_scale      77.04
_oxford_refine_ls_r_factor_ref   0.1098
_oxford_refine_ls_scale          0.08240(4)
_oxford_reflns_number_all        9373
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'SK074A_123K_0m in P-1'
_cod_data_source_file            c8dt01338a2.cif
_cod_data_source_block           SK074A_123K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7046379--7046389.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C50 H40 Cl4 Cu1 F6 N2 O1 P3'
_cod_database_code               7046384