A homochiral Zn-Dy heterometallic left-handed helical chain complex without chiral ligands: anion-induced assembly and multifunctional integration.
Liu, Cai-Ming; Zhang, De-Qing; Xiong, Ren-Gen; Hao, Xiang; Zhu, Dao-Ben; Chemical communications (Cambridge, England) 54 (2018) 13379–13382; doi:10.1039/c8cc07468b

data_7122548
_publ_section_title
;
 A homochiral Zn-Dy heterometallic left-handed helical chain complex
 without chiral ligands: anion-induced assembly and multifunctional
 integration.
;
_journal_issue                   95
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13379
_journal_page_last               13382
_journal_paper_doi               10.1039/c8cc07468b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'0.33(C186 H156 Dy3 N24 O48 Zn9), Cl O4, 2(C H4 O)'
_chemical_formula_sum            'C64 H60 Cl Dy N8 O22 Zn3'
_chemical_formula_weight         1687.32
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-03 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.9961(4)
_cell_length_b                   16.9961(4)
_cell_length_c                   19.8792(5)
_cell_measurement_reflns_used    16301
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      2.4410
_cell_volume                     4973.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_data_collection       'Rigaku CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2018)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku sealed tube Saturn724+'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.397
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.9d (Rigaku OD, 2015) '
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2547
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.34
_refine_diff_density_max         3.355
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 3130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7586
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0623P)^2^+8.9202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7356
_reflns_number_total             7586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07468b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7122548--7122549.cif.'
_cod_original_cell_volume        4973.1(3)
_cod_database_code               7122548
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.507
_shelx_estimated_absorpt_t_min   0.380
_olex2_refinement_description
;
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, All O(H) groups
2. Restrained distances
 C32-O11
 1.42 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16),
 C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C32(H32A,H32B,H32C)
3.d Idealised tetrahedral OH refined as rotating group:
 O11(H11)
;
_shelx_res_checksum              46165
_olex2_submission_special_instructions 'No special instructions were received'