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_7713182
_publ_section_title
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 Conformational Dynamicity in a Copper(II) Coordination Complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01213A
_journal_year                    2023
_chemical_formula_moiety         'C19 H19 Cl Cu N3 S, F6 P, H2 O'
_chemical_formula_sum            'C19 H21 Cl Cu F6 N3 O P S'
_chemical_formula_weight         583.41
_chemical_name_systematic        '[CuCl(dpaSMe)]PF6'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-04-22 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0079(3)
_cell_length_b                   18.5616(7)
_cell_length_c                   13.3009(5)
_cell_measurement_reflns_used    33170
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.51
_cell_volume                     2222.20(14)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60578
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         2.194
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.338
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.7951.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1180
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH/water'
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0756P)^2^+4.4428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4258
_reflns_number_total             4569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01213a2.cif
_cod_data_source_block           '[cucl(dpasme)]pf6_greencryst'
_cod_database_code               7713182
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.676
_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, All O(H,H) groups
2.a Free rotating group:
 O(HA,HB)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.c 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)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              30357
_olex2_submission_special_instructions 'No special instructions were received'