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_7059368
_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 Gd2 N6 Ni2 O19, 2(Cl), O'
_chemical_formula_sum            'C26 H42 Cl2 Gd2 N6 Ni2 O20'
_chemical_formula_weight         1261.46
_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   geom
_audit_creation_date             2020-02-04
_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                 105.322(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8573(8)
_cell_length_b                   23.9482(14)
_cell_length_c                   14.3941(8)
_cell_measurement_reflns_used    55213
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      26.289
_cell_measurement_theta_min      1.696
_cell_volume                     4607.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.986
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55213
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.289
_diffrn_reflns_theta_min         1.696
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    3.837
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.085
_refine_diff_density_min         -4.871
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9023
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+23.0690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2064
_refine_ls_wR_factor_ref         0.2301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6146
_reflns_number_total             9023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05686f2.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
;Adding full bibliography for 7059368--7059371.cif.

 Adding full bibliography for 7059368--7059371.cif.
;
_cod_database_code               7059368
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.635
_shelx_estimated_absorpt_t_min   0.597
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups, All O(H) groups, All
  O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5)
 H7AC(0.5)
 Fixed U11: Cl2(0.164171)
 Fixed U12: Cl2(-0.000304)
 Fixed U13: Cl2(-0.016249)
 Fixed U22: Cl2(0.15699)
 Fixed U23: Cl2(-0.0026)
 Fixed U33: Cl2(0.17579)
4.a Ternary CH refined with riding coordinates:
 O4(H4A), O3(H3C)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C8(H8), C12(H12), C14(H14), C3(H3), C5(H5), C13(H13), C4(H4), N5(H5A),
  C17(H17)
4.c X=CH2 refined with riding coordinates:
 N6(H6A,H6B), O17(H17A,H17B), O18(H18A,H18B), N3(H3A,H3B), O19(H19A,H19B)
4.d 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), C7A(H7AA,H7AB,H7AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98339
_shelx_fab_checksum              82889
_olex2_submission_special_instructions 'No special instructions were received'