Conformational Dynamicity in a Copper(II) Coordination Complex
Griffin, Paul Joseph; Dake, Matthew J.; Remolina, Alesandro D.; Olshansky, Lisa; Dalton Transactions  (2023) –; doi:10.1039/D3DT01213A

data_7713181
_publ_section_title
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 Conformational Dynamicity in a Copper(II) Coordination Complex
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01213A
_journal_year                    2023
_chemical_formula_moiety
'C19 H19 Cl Cu N3 S, 0.25(C Cl2), 1.5(C H2 Cl2), F6 P'
_chemical_formula_sum            'C20.75 H22 Cl4.5 Cu F6 N3 P S'
_chemical_formula_weight         713.51
_chemical_name_systematic        '[CuCl(dpaSMe)]PF6'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
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2023-04-22 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                69.367(2)
_cell_angle_beta                 88.157(2)
_cell_angle_gamma                73.3880(10)
_cell_formula_units_Z            4
_cell_length_a                   11.4469(5)
_cell_length_b                   14.3440(7)
_cell_length_c                   19.0859(9)
_cell_measurement_reflns_used    40044
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.26
_cell_volume                     2802.1(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81376
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.612
_diffrn_reflns_theta_min         2.062
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1106 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.8611.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1432
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.376
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.196
_refine_diff_density_max         2.131
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0568
_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^)+(0.1089P)^2^+5.0434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11377
_reflns_number_total             12905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01213a2.cif
_cod_data_source_block           '[cucl(dpasme)]pf6_bluecrystals'
_cod_original_formula_sum        'C20.75 H22 Cl4.50 Cu F6 N3 P S'
_cod_database_code               7713181
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.621
_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. Others
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F13)=Sof(F16)=Sof(F17)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F12)=Sof(F14)=Sof(F15)=Sof(F18)=FVAR(1)
 Fixed Sof: C20(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C26(H26A,H26B), C27(H27A,H27B), C01X(H01A,H01B),
 C022(H02C,H02D)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24),
  C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C39(H39B,H39A,H39C)
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_shelx_res_checksum              3663
_olex2_submission_special_instructions 'No special instructions were received'