Ligand-dependent formation of ion-pair Cu(I)/Cu(III) trifluoromethyl complexes containing bisphosphines.
Zhang, Song-Lin; Bie, Wen-Feng; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17588–17592; doi:10.1039/c6dt03016e

data_7040516
_publ_section_title
;
 Ligand-dependent formation of ion-pair Cu(I)/Cu(III) trifluoromethyl
 complexes containing bisphosphines.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17588
_journal_page_last               17592
_journal_paper_doi               10.1039/c6dt03016e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C52 H48 Cu P4, C4 Cu F12, C H2 Cl2'
_chemical_formula_sum            'C57 H50 Cl2 Cu2 F12 P4'
_chemical_formula_weight         1284.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-20
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2016-08-24 deposited with the CCDC.
2016-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.568(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5621(10)
_cell_length_b                   15.2407(11)
_cell_length_c                   25.3334(16)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.74
_cell_volume                     5616.8(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62209
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.180
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_T_max  0.8184
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.279
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         12912
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.1087
_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^)+74.0416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2327
_refine_ls_wR_factor_ref         0.2394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10591
_reflns_number_total             12912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03016e2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7040516.cif.'
_cod_database_code               7040516
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 Cl1_1-C1_1 = Cl2_1-C1_1
 Cl1_2-C1_2 = Cl2_2-C1_2
 1.771 with sigma of 0.01
 Cl1_1-Cl2_1
 Cl1_2-Cl2_2
 2.916 with sigma of 0.03
 F10-F11 \\sim F10-F12 \\sim F10A-F11A \\sim F10A-F12A \\sim F11-F12 \\sim
F11A-F12A
 with sigma of 0.04
 Cu2-C54A \\sim Cu2-C54
 with sigma of 0.02
 Cu2-C55 \\sim Cu2-C55A
 with sigma of 0.02
 Cu2-C53A \\sim Cu2-C53
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1_1 \\sim Cl2_1 \\sim C1_1 \\sim Cl1_2 \\sim Cl2_2 \\sim C1_2: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(Cl2_2) = Uanis(Cl1_1)
Uanis(C1_2) = Uanis(C1_1)
4. Rigid body (RIGU) restrains
 Cl1_1, Cl2_1, C1_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1_2, Cl2_2, C1_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu2, C53, C54, C55, C56A, F1A, F2, F3A, F4, F5, F6, F8, F9, F7, F10A, F11A,
 F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu2, C53A, C54A, C55A, C56A, F1, F2A, F3, F4A, F5A, F6A, F7A, F8, F9A, F12,
 F11, F10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F1(0.5) F1A(0.5) F2(0.5) F2A(0.5) F3(0.5) F3A(0.5) F4(0.5)
 F4A(0.5) F5(0.5) F5A(0.5) F6(0.5) F6A(0.5) F7(0.5) F7A(0.5) F9(0.5) F9A(0.5)
 F10(0.5) F10A(0.5) F11(0.5) F11A(0.5) F12(0.5) F12A(0.5) C53A(0.5) C53(0.5)
 C54(0.5) C54A(0.5) C55(0.5) C55A(0.5) Cl1(0.5) Cl2(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) Cl1(0.5) Cl2(0.5) C1(0.5) H1A(0.5) H1B(0.5)
 Fixed Uiso: H2(0.043) H3(0.059) H4(0.058) H5(0.058) H6(0.051) H8(0.031)
 H9(0.039) H10(0.037) H11(0.041) H12(0.032) H13A(0.026) H13B(0.026) H14A(0.029)
 H14B(0.029) H16(0.063) H17(0.081) H18(0.049) H19(0.045) H20(0.035) H22(0.027)
 H23(0.035) H24(0.039) H25(0.043) H26(0.037) H28(0.044) H29(0.062) H30(0.072)
 H31(0.072) H32(0.051) H34(0.047) H35(0.059) H36(0.066) H37(0.056) H38(0.04)
 H39A(0.031) H39B(0.031) H40A(0.029) H40B(0.029) H42(0.039) H43(0.047)
 H44(0.048) H45(0.049) H46(0.041) H48(0.057) H49(0.083) H50(0.066) H51(0.064)
 H52(0.047)
 Fixed X: H2(1.2887) H3(1.3369) H4(1.4833) H5(1.583301) H6(1.5372) H8(1.5046)
 H9(1.6169) H10(1.641101) H11(1.5487) H12(1.436599) H13A(1.353601) H13B(1.4172)
 H14A(1.2904) H14B(1.2716) H16(1.1494) H17(1.0224) H18(0.8775) H19(0.856)
 H20(0.982399) H22(1.178101) H23(1.169801) H24(1.1449) H25(1.124701)
 H26(1.1335) H28(0.9412) H29(0.8353) H30(0.8849) H31(1.0352) H32(1.1355)
 H34(1.0855) H35(1.163701) H36(1.317101) H37(1.3998) H38(1.320901) H39A(1.1078)
 H39B(1.0151) H40A(1.0355) H40B(1.0545) H42(1.323601) H43(1.3834) H44(1.351301)
 H45(1.264) H46(1.198701) H48(1.325101) H49(1.329301) H50(1.1926) H51(1.058201)
 H52(1.0514)
 Fixed Y: H2(0.0909) H3(0.014) H4(-0.0366) H5(-0.0183) H6(0.0568) H8(0.243)
 H9(0.3397) H10(0.362901) H11(0.292) H12(0.1941) H13A(-0.0078) H13B(0.047)
 H14A(0.111301) H14B(0.0097) H16(0.0742) H17(0.0728) H18(0.076699) H19(0.0881)
 H20(0.0871) H22(-0.108999) H23(-0.2359) H24(-0.2322) H25(-0.0997)
 H26(0.029301) H28(0.2196) H29(0.125001) H30(0.020901) H31(0.022) H32(0.125001)
 H34(0.3606) H35(0.4278) H36(0.4073) H37(0.318901) H38(0.2529) H39A(0.3994)
 H39B(0.3471) H40A(0.2953) H40B(0.3968) H42(0.3696) H43(0.4991) H44(0.6302)
 H45(0.627601) H46(0.499599) H48(0.3321) H49(0.3296) H50(0.3146) H51(0.3008)
 H52(0.313801)
 Fixed Z: H2(0.1326) H3(0.0594) H4(0.058301) H5(0.129601) H6(0.204) H8(0.1871)
 H9(0.2186) H10(0.308001) H11(0.3665) H12(0.3357) H13A(0.2651) H13B(0.304399)
 H14A(0.3425) H14B(0.3414) H16(0.3929) H17(0.444599) H18(0.406699) H19(0.3165)
 H20(0.2635) H22(0.3051) H23(0.2573) H24(0.1665) H25(0.124101) H26(0.1722)
 H28(0.166901) H29(0.1265) H30(0.0677) H31(0.042399) H32(0.0778) H34(0.0696)
 H35(0.003201) H36(-0.0041) H37(0.0576) H38(0.124801) H39A(0.1768) H39B(0.1725)
 H40A(0.2591) H40B(0.2622) H42(0.1998) H43(0.1704) H44(0.212399) H45(0.2858)
 H46(0.313201) H48(0.3584) H49(0.4492) H50(0.493) H51(0.445999) H52(0.3549)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1(H1A,H1B)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.680
_shelx_res_checksum              65104
_shelx_shelxl_version_number     2014/7