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_7059370
_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 Ho2 N6 Ni2 O19, 2(Cl), H2 O'
_chemical_formula_sum            'C26 H42 Cl2 Ho2 N6 Ni2 O20'
_chemical_formula_weight         1276.83
_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                 100.79
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.421
_cell_length_b                   23.686
_cell_length_c                   14.348
_cell_measurement_reflns_used    38048
_cell_measurement_temperature    295.97
_cell_measurement_theta_max      27.508
_cell_measurement_theta_min      2.914
_cell_volume                     4480.443
_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      295.97
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_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  0.0646
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38048
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         2.876
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.516
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1113 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.4338.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.557
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         9920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+4.5119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7454
_reflns_number_total             9920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05686f2.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
;Adding full bibliography for 7059368--7059371.cif.

 Adding full bibliography for 7059368--7059371.cif.
;
_cod_original_cell_volume        4480.4
_cod_database_code               7059370
_shelx_shelxl_version_number     2018/3
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O0AA(H0AA,H0AB)
2.b Rotating group:
 O17(H17A,H17B), O18(H18A,H18B), N6(H6A,H6B), N3(H3A,H3B), O19(H19A,H19B)
2.c Ternary CH refined with riding coordinates:
 O4(H4), O3(H3)
2.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C17(H17), C8(H8), C14(H14), C13(H13), C12(H12), C4(H4A),
 C3(H3C), C5(H5A)
2.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), 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              78356
_shelx_fab_checksum              38077
_olex2_submission_special_instructions 'No special instructions were received'