[Cu(POP)(N^S)][PF6] and [Cu(xantphos)(N^S)][PF6] compounds with 2-(thiophen-2-yl)pyridines
Nohara, Isaak; Prescimone, Alessandro; Häussinger, Daniel; Housecroft, Catherine E.; Constable, Edwin C.; RSC Advances 9 (2019) 13646–; doi:10.1039/C9RA02617G

data_7232714
_publ_section_title
;
 [Cu(POP)(N^S)][PF6] and [Cu(xantphos)(N^S)][PF6] compounds with
 2-(thiophen-2-yl)pyridines
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              13646
_journal_paper_doi               10.1039/C9RA02617G
_journal_volume                  9
_journal_year                    2019
_chemical_compound_source        'Isaak Nohara'
_chemical_formula_moiety         'C48 H39 Cu1 F6 N1 O1 P3 S1'
_chemical_formula_sum            'C48 H39 Cu F6 N O P3 S'
_chemical_formula_weight         948.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2018-02-05
_audit_creation_method           CRYSTALS_ver_14.61_build_6720
_audit_update_record
;
2019-03-01 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.118(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5055(13)
_cell_length_b                   21.487(3)
_cell_length_c                   19.094(2)
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    123
_cell_measurement_theta_max      70
_cell_measurement_theta_min      3
_cell_volume                     4292.9(9)
_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 0.986
_diffrn_measured_fraction_theta_max 0.954
_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  0.033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56802
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         70.234
_diffrn_reflns_theta_min         3.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.785
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_recrystallization_method
; 
DCM / Et2O
;
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.23
_refine_diff_density_min         -1.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9592
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         7742
_refine_ls_number_restraints     690
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.0018078
_refine_ls_shift/su_mean         0.0000492
_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: 
 1.96 2.46 0.678 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0877
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0877
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7732
_reflns_number_total             7797
_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   0.0505
_oxford_refine_ls_scale          0.079960(12)
_oxford_reflns_number_all        7742
_oxford_structure_analysis_title 'ISN109_123K_0m in P2(1)/c'
_cod_data_source_file            c9ra02617g2.cif
_cod_data_source_block           ISN109_123K
_cod_original_cell_volume        4293.0(9)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C48 H39 Cu1 F6 N1 O1 P3 S1'
_cod_database_code               7232714
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)