Substituents Lead to Differences in the Formation of Two Different Butterfly-shaped NiⅡ2DyⅢ2 Clusters: Structures and Multistep Assembly Mechanisms
Mo, Kai-Qiang; Zhu, Zhonghong; Wang, Hai-Ling; Ma, Xiong-Feng; Peng, Jin-Mei; Zou, Hua-Hong; Bai, Juan; Liang, Fu-Pei; Dalton Transactions  (2019) –; doi:10.1039/C9DT03795K

data_7701383
_publ_section_title
;
 Substituents Lead to Differences in the Formation of Two Different
 Butterfly-shaped Ni&#x2161;2Dy&#x2162;2 Clusters: Structures and
 Multistep Assembly Mechanisms
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03795K
_journal_year                    2019
_chemical_formula_moiety         'C42 H54 Dy2 N8 Ni2 O22, 0.67(O3)'
_chemical_formula_sum            'C42 H54 Dy2 N8 Ni2 O24'
_chemical_formula_weight         1497.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-15 deposited with the CCDC.    2019-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.760(6)
_cell_length_b                   13.880(3)
_cell_length_c                   16.570(3)
_cell_measurement_temperature    293(2)
_cell_volume                     6130(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4869
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.093
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2968
_refine_diff_density_max         2.141
_refine_diff_density_min         -2.282
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         4869
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1521P)^2^+47.8046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                4847
_reflns_number_total             4869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt03795k2.cif
_cod_data_source_block           tt
_cod_database_code               7701383
_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
C12 \\sim C18 \\sim C7 \\sim C9 \\sim C8 \\sim C14 \\sim C3 \\sim C17 \\sim C13
\\sim C19 \\sim C10 \\sim C15 \\sim C16 \\sim C1 \\sim C11 \\sim C5 \\sim C20
\\sim C21 \\sim C6 \\sim C2 \\sim C4: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O7) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O13(0.33333) O14(0.33333) O12(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C14(H14), C19(H19), C15(H15), C16(H16), C5(H5), C6(H6), C4(H4)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'