;   () –; doi:10.1039/D4CP04569F

data_1573815
_journal_paper_doi               10.1039/D4CP04569F
_chemical_formula_moiety         'C32 H46 Cl4 Cu2 N8 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C36 H52 Cl4 Cu2 N10 O16'
_chemical_formula_weight         1149.75
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-09-05 deposited with the CCDC.	2025-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.215(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.628(4)
_cell_length_b                   8.5678(18)
_cell_length_c                   15.791(3)
_cell_measurement_reflns_used    4437
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.31
_cell_volume                     2381.2(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1656
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29525
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.314
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5080
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Block
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       Blue
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4205
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2664
_reflns_number_total             4205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp04569f3.cif
_cod_data_source_block           Cu2L2B8
_cod_original_cell_volume        2381.2(8)
_cod_database_code               1573815
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.893
_olex2_refinement_description
;
1. Restrained distances
 Cl2-O5 \\sim Cl2-O5A
 with sigma of 0.02
 Cu1-N2 \\sim Cu1-N2A
 with sigma of 0.02
 Cl2-O6 \\sim Cl2-O6A
 with sigma of 0.02
 N2-C6 \\sim N2A-C6
 with sigma of 0.02
 N2-C7 \\sim N2A-C7
 with sigma of 0.02
 Cl2-O7 \\sim Cl2-O7A
 with sigma of 0.02
 Cl2-O8 \\sim Cl2-O8A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O7A) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(O8A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O6) = Uanis(O6A)
Uanis(O8A) = Uanis(O8)
Uanis(O5A) = Uanis(O5)
Uanis(O7A) = Uanis(O7)
3. Others
 Sof(O7A)=Sof(O5A)=Sof(O8A)=Sof(O6A)=1-FVAR(1)
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Sof(H6BC)=Sof(H6BD)=Sof(H7BC)=Sof(H7BD)=Sof(N2A)=Sof(H2AA)=1-FVAR(2)
 Sof(N2)=Sof(H2)=Sof(H6AA)=Sof(H6AB)=Sof(H7AA)=Sof(H7AB)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 N2(H2), N2A(H2AA)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6AA,H6AB), C6(H6BC,H6BD), C7(H7AA,H7AB), C7(H7BC,H7BD), N4(H4A,H4B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              95782
_olex2_submission_special_instructions 'No special instructions were received'