Coordination control of a semicarbazide Schiff base ligand for spontaneous aggregation of a Ni2Ln2 cubane family: influence of ligand arms and carboxylate bridges on the organization of the magnetic core
Biswas, Mousumi; Sañudo, E. Carolina; Cirera, Jordi; Ray, Debashis; New Journal of Chemistry 44 (2020) 4812–4821; doi:10.1039/C9NJ05686F

data_7059369
_publ_section_title
;
 Coordination control of a semicarbazide Schiff base ligand for
 spontaneous aggregation of a Ni2Ln2 cubane family: influence of ligand
 arms and carboxylate bridges on the organization of the magnetic core
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4812
_journal_page_last               4821
_journal_paper_doi               10.1039/C9NJ05686F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C26 H40 Dy2 N6 Ni2 O19, 2(Cl), O'
_chemical_formula_sum            'C26 H42 Cl2 Dy2 N6 Ni2 O20'
_chemical_formula_weight         1271.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-02-05
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-07 deposited with the CCDC.	2020-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.61(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.419(17)
_cell_length_b                   23.74(3)
_cell_length_c                   14.18(3)
_cell_measurement_reflns_used    44294
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.177
_cell_measurement_theta_min      2.257
_cell_volume                     4390(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44294
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.141
_diffrn_reflns_theta_min         1.708
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.407
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.891
_refine_diff_density_min         -4.567
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9236
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1264P)^2^+20.1659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2168
_refine_ls_wR_factor_ref         0.2458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5816
_reflns_number_total             9236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05686f2.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
;Adding full bibliography for 7059368--7059371.cif.

 Adding full bibliography for 7059368--7059371.cif.
;
_cod_original_cell_volume        4392(12)
_cod_database_code               7059369
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H18A,H18B} of O18, {H17A,H17B} of O17, All N(H) groups,
  All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H19A,H19B} of O19
2. Restrained distances
 Dy2-H19A \\sim Dy2-H19B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed U11: Cl2(0.207679)
 Fixed U12: Cl2(0.017814)
 Fixed U13: Cl2(-0.035141)
 Fixed U22: Cl2(0.21194)
 Fixed U23: Cl2(0.01312)
 Fixed U33: Cl2(0.21329)
5.a Free rotating group:
 O19(H19A,H19B)
5.b Ternary CH refined with riding coordinates:
 O3(H3), O4(H4)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C17(H17), C8(H8), C14(H14), C13(H13), C12(H12), C3(H3C),
 C5(H5A), C4(H4A)
5.d X=CH2 refined with riding coordinates:
 O17(H17A,H17B), N3(H3A,H3B), N6(H6A,H6B), O18(H18A,H18B)
5.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C7(H7A,H7B,H7C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74594
_shelx_fab_checksum              35563
_olex2_submission_special_instructions 'No special instructions were received'