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_7701384
_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         'C40 H48 N16 Na2 Ni2 O8'
_chemical_formula_sum            'C40 H48 N16 Na2 Ni2 O8'
_chemical_formula_weight         1044.34
_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             2019-06-03
_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                 123.044(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.989(6)
_cell_length_b                   11.319(3)
_cell_length_c                   20.032(5)
_cell_measurement_reflns_used    6290
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.77
_cell_measurement_theta_min      2.43
_cell_volume                     4750(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26872
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stripe
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4645
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.365
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0718P)^2^+7.7188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                3543
_reflns_number_total             4645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt03795k2.cif
_cod_data_source_block           1
_cod_database_code               7701384
_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. Restrained distances
 C1-Na1
 2 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C19(H19a,H19b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C13(H13), C14(H14), C15(H15), C17(H17)
3.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C18(H18a,H18b,H18c), C20(H20a,H20b,H20c)
;
_olex2_submission_special_instructions 'No special instructions were received'