[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_7232709
_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         'C46 H37 Cu N O P2 S, F6 P, C H2 Cl2'
_chemical_formula_sum            'C47 H39 Cl2 Cu F6 N O P3 S'
_chemical_formula_weight         1007.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-04
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-01 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                71.646(3)
_cell_angle_beta                 75.679(3)
_cell_angle_gamma                70.826(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5738(10)
_cell_length_b                   12.4356(12)
_cell_length_c                   18.8853(17)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    130
_cell_measurement_theta_max      70.027
_cell_measurement_theta_min      3.893
_cell_volume                     2197.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28575
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.241
_diffrn_reflns_theta_min         3.892
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.5712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0920 before and 0.0347 after correction.
The Ratio of minimum to maximum transmission is 0.7583.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       needle
_exptl_crystal_F_000             1028
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DCM and Et2O  by solvent layering'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.439
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         7961
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+3.6381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7776
_reflns_number_total             7961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra02617g2.cif
_cod_data_source_block           isn127_130k_0m
_cod_database_code               7232709
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.391
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim C41 \\sim C40 \\sim C39 \\sim C38 \\sim C37: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
S1 \\sim N2 \\sim C42 \\sim C41 \\sim C37 \\sim C44 \\sim C39 \\sim C40 \\sim
C38 \\sim C43 \\sim C45 \\sim C46: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C46A \\sim C45A \\sim C44A \\sim C43A \\sim C42A \\sim S2 \\sim C41A \\sim N1
\\sim C37A \\sim C38A \\sim C39A \\sim C40A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(N2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(S1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C46A) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C44A) \\sim Ueq,
Uanis(C43A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(C41A)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(C39A) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 C46, C45, S1, C44, C43, C42, C41, C40, C39, C38, C37, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, C42A, C43A, C44A, C45A, C46A, C41A, C40A, C39A, C38A, C37A, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: S1(0.8) N2(0.8) C42(0.8) C41(0.8) C37(0.8) H37(0.8) C44(0.8)
 H44(0.8) C39(0.8) H39(0.8) C40(0.8) H40(0.8) C38(0.8) H38(0.8) C43(0.8)
 H43(0.8) C45(0.8) C46(0.8) H46A(0.8) H46B(0.8) H46C(0.8) C46A(0.2) H46D(0.2)
 H46E(0.2) H46F(0.2) C45A(0.2) C44A(0.2) H44A(0.2) C43A(0.2) H43A(0.2)
 C42A(0.2) S2(0.2) C41A(0.2) N1(0.2) C37A(0.2) H37A(0.2) C38A(0.2) H38A(0.2)
 C39A(0.2) H39A(0.2) C40A(0.2) H40A(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C23(H23), C8(H8), C32(H32), C20(H20), C30(H30), C28(H28), C22(H22),
 C14(H14), C6(H6), C36(H36), C12(H12), C21(H21), C2(H2), C27(H27), C16(H16),
 C29(H29), C9(H9), C11(H11), C17(H17), C15(H15), C34(H34), C5(H5), C10(H10),
 C35(H35), C37(H37), C3(H3), C33(H33), C44(H44), C39(H39), C40(H40), C38(H38),
 C4(H4), C43(H43), C44A(H44A), C43A(H43A), C37A(H37A), C38A(H38A), C39A(H39A),
 C40A(H40A)
5.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C46A(H46D,H46E,H46F)
;
_shelx_res_checksum              15447
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'