[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_7232710
_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         'C50 H43 Cu N O P2 S, F6 P'
_chemical_formula_sum            'C50 H43 Cu F6 N O P3 S'
_chemical_formula_weight         976.36
_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             2019-01-22
_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                82.221(3)
_cell_angle_beta                 71.606(3)
_cell_angle_gamma                88.977(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5350(5)
_cell_length_b                   12.1924(6)
_cell_length_c                   17.0548(8)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      69.698
_cell_measurement_theta_min      4.040
_cell_volume                     2254.30(19)
_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 0.985
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27121
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.090
_diffrn_reflns_theta_min         2.756
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.668
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0749 before and 0.0490 after correction.
The Ratio of minimum to maximum transmission is 0.8746.
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    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_recrystallization_method 'DCM / Et2O'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.739
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0901P)^2^+3.6669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6150
_reflns_number_total             8187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra02617g2.cif
_cod_data_source_block           isn147_130k_0m
_cod_database_code               7232710
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C36(H36), C35(H35), C50(H50), C34(H34), C25(H25), C26(H26),
 C23(H23), C13(H13), C44(H44), C40(H40), C27(H27), C46(H46), C21(H21), C49(H49),
  C14(H14), C20(H20), C15(H15), C17(H17), C48(H48), C41(H41), C47(H47),
 C42(H42), C22(H22), C43(H43), C7(H7), C16(H16), C9(H9), C4(H4), C3(H3), C8(H8)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              10985
_olex2_submission_original_sample_id ISN417_130K
_olex2_submission_special_instructions 'No special instructions were received'