Heterodinuclear [Co-Ln] complexes of semicarbazide-arm bearing ligand: synthesis from the cleavage of starting [Co-Co] complex, structures and magnetic properties
Biswas, Mousumi; Basak, Dipmalya; Sañudo, E. Carolina; Ray, Debashis; New Journal of Chemistry 45 (2021) 8755–8762; doi:10.1039/D1NJ00971K

data_7060555
_publ_section_title
;
 Heterodinuclear [Co-Ln] complexes of semicarbazide-arm bearing ligand:
 synthesis from the cleavage of starting [Co-Co] complex, structures and
 magnetic properties
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8755
_journal_page_last               8762
_journal_paper_doi               10.1039/D1NJ00971K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C30 H50 Co Ho N3 O12, 3(C H4 O)'
_chemical_formula_sum            'C33 H62 Co Ho N3 O15'
_chemical_formula_weight         964.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-04
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-04-03 deposited with the CCDC.	2021-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            4
_cell_length_a                   22.550(5)
_cell_length_b                   10.051(2)
_cell_length_c                   18.174(4)
_cell_measurement_reflns_used    9598
_cell_measurement_temperature    156.15
_cell_measurement_theta_max      26.927
_cell_measurement_theta_min      2.443
_cell_volume                     4119.1(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      156.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52955
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         1.806
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.377
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       plate
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.177(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8580
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+7.3154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.890
_reflns_Friedel_fraction_max     0.829
_reflns_number_gt                8199
_reflns_number_total             8580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00971k2.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
'Adding full bibliography for 7060553--7060556.cif.'
_cod_database_code               7060555
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.823(11)
 0.177(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H12 of O12, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14 of O14, H15 of O15, H13 of O13
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 O12(H12), N2(H2), C7(H7), C3(H3), C5(H5), C4(H4)
4.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C32(H32A,H32B,H32C), C18(H18A,
 H18B,H18C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C24(H24A,H24B,H24C),
 C33(H33A,H33B,H33C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,
 H31C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C)
4.d Idealised tetrahedral OH refined as rotating group:
 O14(H14), O13(H13), O15(H15)
;
_shelx_res_checksum              30866
_olex2_submission_special_instructions 'No special instructions were received'