Chimera Diimine Ligands in Emissive [Cu(P^P)(N^N)][PF6] Complexes
Meyer, Marco; Brunner, Fabian; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; Inorganics 8 (2020) 33–; doi:10.3390/inorganics8050033

data_1558185
_publ_section_title
;
 Chimera Diimine Ligands in Emissive [Cu(P^P)(N^N)][PF6] Complexes
;
_journal_issue                   5
_journal_name_full               Inorganics
_journal_page_first              33
_journal_paper_doi               10.3390/inorganics8050033
_journal_volume                  8
_journal_year                    2020
_chemical_compound_source        'Marco Meyer'
_chemical_formula_moiety         'C47 H37 Cl1 Cu1 F6 N2 O1 P3'
_chemical_formula_sum            'C47 H37 Cl Cu F6 N2 O P3'
_chemical_formula_weight         951.73
_chemical_melting_point          ?
_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     other
_audit_creation_date             2018-10-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6949
_cell_angle_alpha                90
_cell_angle_beta                 100.077(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4786(3)
_cell_length_b                   18.9864(4)
_cell_length_c                   22.1096(5)
_cell_measurement_reflns_used    4110
_cell_measurement_temperature    130
_cell_measurement_theta_max      57
_cell_measurement_theta_min      3
_cell_volume                     4330.87(18)
_computing_cell_refinement       'STOE X-AREA (Stoe & Cie 2011)'
_computing_data_collection       'STOE X-AREA (Stoe & Cie 2011)'
_computing_data_reduction        'STOE X-RED (Stoe & Cie 1996)'
_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      130
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48628
_diffrn_reflns_theta_full        54.895
_diffrn_reflns_theta_max         57.183
_diffrn_reflns_theta_min         2.687
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_voltage           70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.150
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_recrystallization_method
; 
Acetone / Hexane
;
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.39
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0315
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         7217
_refine_ls_number_restraints     668
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.1124
_refine_ls_shift/su_max          0.0004785
_refine_ls_shift/su_mean         0.0000225
_refine_ls_structure_factor_coef F
_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: 
 0.218 -0.653 -0.909E-02 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0443
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0443
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7234
_reflns_number_total             8755
_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   0.1126
_oxford_refine_ls_scale          0.3225(4)
_oxford_reflns_number_all        7234
_oxford_structure_analysis_title 'MEM011_130K in P 21/n'
_cod_data_source_file            MEM011_130K.cif
_cod_data_source_block           MEM011_130K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C47 H37 Cl1 Cu1 F6 N2 O1 P3'
_cod_database_code               1558185
_oxford_refine_reflns_threshold_expression_ref I>2.0\s(I)