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_7122549
_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         'C86 H64 Dy2 N12 O24 Zn3'
_chemical_formula_sum            'C86 H64 Dy2 N12 O24 Zn3'
_chemical_formula_weight         2170.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-30
_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                90
_cell_formula_units_Z            8
_cell_length_a                   16.007(3)
_cell_length_b                   21.007(4)
_cell_length_c                   55.589(11)
_cell_measurement_reflns_used    33348
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4847
_cell_measurement_theta_min      6.5625
_cell_volume                     18692(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0720
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            111682
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.433
_diffrn_reflns_theta_min         0.733
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.60629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       block
_exptl_crystal_F_000             8624
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         21239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1021P)^2^+158.4775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19600
_reflns_number_total             21239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07468b2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7122548--7122549.cif.'
_cod_original_cell_volume        18693(6)
_cod_database_code               7122549
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.390
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C43) = Uanis(C43')
3. Others
 Sof(C43')=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B)
4.b Me refined with riding coordinates:
 C43(H43A,H43B,H43C), C43'(H43D,H43E,H43F)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29), C32(H32),
  C36(H36), C38(H38), C39(H39), C40(H40), C46(H46), C47(H47), C48(H48),
 C51(H51), C55(H55), C57(H57), C58(H58), C59(H59), C65(H65), C66(H66), C67(H67),
  C70(H70), C71(H71), C72(H72), C77(H77), C78(H78), C79(H79), C82(H82),
 C83(H83), C84(H84)
4.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C44(H44A,H44B,H44C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              62777
_shelx_fab_checksum              75136
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'