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

data_7709908
_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_absolute_configuration ad
_chemical_formula_moiety         'C38 H38 Cl Cu2 N6 O2, Cl2 Cu'
_chemical_formula_sum            'C38 H38 Cl3 Cu3 N6 O2'
_chemical_formula_weight         907.71
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-14
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2127(2)
_cell_length_b                   19.9564(5)
_cell_length_c                   23.1694(6)
_cell_measurement_reflns_used    10218
_cell_measurement_temperature    130.0
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      2.223
_cell_volume                     3797.37(17)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28242
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         2.033
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6479
_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 0.0851 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.8692.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       plates
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 2791 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(7)
_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     471
_refine_ls_number_reflns         7769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0198P)^2^+0.7511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0596
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7055
_reflns_number_total             7769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00312k2.cif
_cod_data_source_block           dpaomecucl
_cod_database_code               7709908
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.652
_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:
 C25(H25A,H25B), C33(H33A,H33B), C6(H6A,H6B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C29(H29), C30(H30), C36(H36), C9(H9), C28(H28), C10(H10), C22(H22),
 C23(H23), C4(H4), C1(H1), C35(H35), C2(H2), C18(H18), C21(H21), C27(H27),
 C20(H20), C12(H12), C3(H3), C16(H16), C38(H38), C11(H11), C37(H37), C17(H17)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C32(H32A,H32B,H32C)
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_olex2_submission_special_instructions 'No special instructions were received'