Conformationally dynamic copper coordination complexes
Charette, Bronte J.; Griffin, Paul J.; Zimmerman, Claire M.; Olshansky, Lisa; Dalton Transactions  (2022) –; doi:10.1039/D2DT00312K

data_7709909
_publ_section_title
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 Conformationally dynamic copper coordination complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00312K
_journal_year                    2022
_chemical_formula_moiety         'C19 H19 Cl Cu N3 O, 2(C H2 Cl2), F6 P'
_chemical_formula_sum            'C21 H23 Cl5 Cu F6 N3 O P'
_chemical_formula_weight         719.18
_chemical_name_systematic        '[CuClDPA]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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2022-01-28 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
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_cell_angle_alpha                72.920(2)
_cell_angle_beta                 69.922(2)
_cell_angle_gamma                78.631(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4034(6)
_cell_length_b                   11.1847(7)
_cell_length_c                   13.3875(7)
_cell_measurement_reflns_used    9137
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      2.25
_cell_volume                     1390.49(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  0.0399
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            50209
_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         26.491
_diffrn_reflns_theta_min         1.916
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0589 after correction.
The Ratio of minimum to maximum transmission is 0.8654.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       Prism
_exptl_crystal_F_000             722
_exptl_crystal_recrystallization_method
'obtained via vapor diffusion of pentane into DCM.'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.336
_exptl_crystal_size_min          0.164
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0684P)^2^+3.8636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5057
_reflns_number_total             5716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00312k2.cif
_cod_data_source_block           '[cucldpa]pf6'
_cod_database_code               7709909
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.600
_olex2_refinement_description
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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.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C20(H20A,H20B), C21(H21A,H21B)
2.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)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
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_shelx_res_checksum              13965
_shelx_hkl_checksum              89357
_olex2_exptl_crystal_mounting_method mounted
_olex2_submission_special_instructions 'No special instructions were received'