Organoamine-induced isomerism of calixarene-based complexes: from 1D to 2D
Zhu, Xiaofei; Wang, Shentang; Han, Haitao; Liao, Wuping; RSC Advances 8 (2018) 39208–; doi:10.1039/C8RA07833E

data_7231861
_publ_section_title
;
 Organoamine-induced isomerism of calixarene-based complexes: from 1D to
 2D
;
_journal_issue                   68
_journal_name_full               'RSC Advances'
_journal_page_first              39208
_journal_paper_doi               10.1039/C8RA07833E
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         '0.5(C144 H124 Cl2 Co8 N12 O24 S8)'
_chemical_formula_sum            'C72 H62 Cl Co4 N6 O12 S4'
_chemical_formula_weight         1602.68
_chemical_name_common
'[Co4 Cl (C40 H44 S4 O4) (C16 H9 N3 O4)2](CH3)4N '
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5565)
;
_audit_update_record
;
2018-11-15 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.549(3)
_cell_length_b                   20.549(3)
_cell_length_c                   15.790(3)
_cell_measurement_reflns_used    6859
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      33.57
_cell_measurement_theta_min      2.80
_cell_volume                     6667.5(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      189.99
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1684
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17571
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        33.905
_diffrn_reflns_theta_max         33.905
_diffrn_reflns_theta_min         2.798
_exptl_absorpt_coefficient_mu    4.887
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.3609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.798
_exptl_crystal_description       block
_exptl_crystal_F_000             1642
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         1322
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0509
_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^)+16.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.626
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                901
_reflns_number_total             1322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra07833e2.cif
_cod_data_source_block           2d-co
_cod_original_cell_volume        6667(2)
_cod_database_code               7231861
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.85(2)
 0.15(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C14, C1, C2, C6, O0AA, C3, C5, S1, Co1, C4, O1AA, Cl1, C7, C11, C8, C9, C10,
 C12, O3, C13, C17, C16, C15, C18, N1, N2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Fixed Sof: H1(0.5)
5.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C14(H14), C16(H16), C17(H17), N1(H1)
5.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C12(C13,C14,C15,C16,C17)
;
_shelx_res_checksum              5490
_shelx_fab_checksum              27059
_olex2_submission_special_instructions 'No special instructions were received'