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_7701382
_publ_section_title
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 Substituents Lead to Differences in the Formation of Two Different
 Butterfly-shaped Ni&#x2161;2Dy&#x2162;2 Clusters: Structures and
 Multistep Assembly Mechanisms
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03795K
_journal_year                    2019
_chemical_formula_moiety         'C38 H40 Dy2 N8 Ni2 O22'
_chemical_formula_sum            'C38 H40 Dy2 N8 Ni2 O22'
_chemical_formula_weight         1403.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-16
_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                 110.65(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.79(3)
_cell_length_b                   13.35(3)
_cell_length_c                   16.23(5)
_cell_measurement_reflns_used    7038
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.03
_cell_volume                     2390(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0875
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21724
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.40
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1114 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.6887.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.027
_refine_diff_density_max         5.603
_refine_diff_density_min         -2.583
_refine_diff_density_rms         0.413
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+52.2937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1957
_refine_ls_wR_factor_ref         0.2368
_reflns_number_gt                3216
_reflns_number_total             4446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt03795k2.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        2390(12)
_cod_database_code               7701382
_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
C9 \\sim C8 \\sim C7 \\sim C6 \\sim C3 \\sim C17 \\sim C5 \\sim C12 \\sim C4
\\sim C19 \\sim C15 \\sim C13 \\sim C16 \\sim C11 \\sim C14 \\sim C10 \\sim C18
\\sim C2 \\sim C1: within 3.8A with sigma of 0.02 and sigma for terminal atoms
of 0.01
Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C5(H5), C4(H4), C15(H15), C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C1(H1A,H1B,H1C)
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_olex2_submission_special_instructions 'No special instructions were received'