[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_7232711
_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         'C43 H38 Cu N2 O P2, F6 P, C2 H5 O0.5'
_chemical_formula_sum            'C45 H43 Cu F6 N2 O1.5 P3'
_chemical_formula_weight         906.26
_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             2019-01-24
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-05 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                110.080(5)
_cell_angle_beta                 99.380(5)
_cell_angle_gamma                102.758(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7193(10)
_cell_length_b                   14.8522(17)
_cell_length_c                   17.864(2)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      70.11
_cell_measurement_theta_min      3.32
_cell_volume                     2280.5(5)
_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      130.0
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0412
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25739
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.289
_diffrn_reflns_theta_min         2.728
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.8293.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       plate
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.511
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         8116
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+6.2950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7338
_reflns_number_total             8116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra02617g2.cif
_cod_data_source_block           isn109_130k_0m
_cod_original_cell_volume        2280.5(4)
_cod_original_formula_sum        'C45 H43 Cu F6 N2 O1.50 P3'
_cod_database_code               7232711
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C47 \\sim C46-C48
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C46) = Uanis(C48) = Uanis(C47)
4. Others
 Fixed Sof: O2(0.5) C46(0.5) H46A(0.25) H46B(0.25) H46C(0.25) H46D(0.25)
 C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C44(0.5) H44A(0.5) H44B(0.5) C47(0.25)
 H47A(0.25) H47B(0.25) H47C(0.25) C48(0.25) H48A(0.25) H48B(0.25) H48C(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C46(H46C,H46D), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C24(H24), C39(H39), C29(H29), C30(H30), C14(H14), C38(H38),
 C23(H23), C36(H36), C35(H35), C33(H33), C9(H9), C12(H12), C37(H37), C8(H8),
 C15(H15), C16(H16), C6(H6), C31(H31), C11(H11), C10(H10), C32(H32), C5(H5),
 C2(H2), C3(H3), C4(H4)
5.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C41(H41A,H41B,
 H41C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              26765
_olex2_submission_special_instructions 'No special instructions were received'