New Supramolecular Heterosynthon [C-I∙∙∙O=C(carboxylate)] at Work: Engineering of the Copper Acetates Cocrystals.
Torubaev, Yury; Skabitskiy, Ivan V.; CrystEngComm  (2020) –; doi:10.1039/D0CE01093F

data_7241158
_publ_section_title
;
 New Supramolecular Heterosynthon
 [C-I&#x2219;&#x2219;&#x2219;O=C(carboxylate)] at Work: Engineering of the
 Copper Acetates Cocrystals.
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01093F
_journal_year                    2020
_chemical_formula_moiety         '4(C3 F2 I), 2(C5 H10 Cu O5), 2(C H4 O)'
_chemical_formula_sum            'C24 H28 Cu2 F8 I4 O12'
_chemical_formula_weight         1295.14
_chemical_name_systematic
'Di-coper(II) tetra-acetate 1,4-diiodo tetrafluorobenzene methanol solvate'
_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             2020-07-19
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-22 deposited with the CCDC.	2020-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.1910(10)
_cell_angle_beta                 98.1120(10)
_cell_angle_gamma                97.8980(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7053(3)
_cell_length_b                   14.5425(5)
_cell_length_c                   15.3896(5)
_cell_measurement_reflns_used    9555
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.56
_cell_volume                     1909.97(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.910
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30709
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.525
_diffrn_reflns_theta_min         2.386
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.437
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0970 before and 0.0478 after correction. The Ratio of minimum to maximum transmission is 0.7256. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.128
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         10634
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0368P)^2^+3.6452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8055
_reflns_number_total             10634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01093f2.cif
_cod_data_source_block           2_CCDC2
_cod_database_code               7241158
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.314
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 O11-H11
 0.85 with sigma of 0.01
 C5-H5
 1.898011 with sigma of 0.02
 Cu1-H5
 2.760451 with sigma of 0.02
 C11-H11
 1.894854 with sigma of 0.02
 Cu2-H11
 2.757623 with sigma of 0.02
 I4-C24 \\sim I4A-C24
 with sigma of 0.02
3. Others
 Sof(I4A)=1-FVAR(1)
 Sof(I4)=FVAR(1)
4.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C)
4.b Idealised tetrahedral OH refined as rotating group:
 O6(H6), O12(H12)
;
_shelx_res_checksum              28962
_olex2_submission_special_instructions 'No special instructions were received'