Ferromagnetically coupled CoII2LnIII2 complexes (where LnIII = Ho, Er, Yb): experimental and theoretical investigations
Ahmed, Naushad; Sahu, Prem Prakash; CrystEngComm 25 (2023) 6592–6601; doi:10.1039/D3CE00827D

data_7247820
_publ_section_title
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 Ferromagnetically coupled CoII2LnIII2 complexes (where LnIII = Ho, Er,
 Yb): experimental and theoretical investigations
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_journal_issue                   47
_journal_name_full               CrystEngComm
_journal_page_first              6592
_journal_page_last               6601
_journal_paper_doi               10.1039/D3CE00827D
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C66 H69 Co2 Ho2 N4 O20, 8(C H4 O), 3(N O3)'
_chemical_formula_sum            'C74 H101 Co2 Ho2 N7 O37'
_chemical_formula_weight         2128.33
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-08-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
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2023-10-16 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.761(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.692(7)
_cell_length_b                   15.981(4)
_cell_length_c                   19.803(5)
_cell_measurement_reflns_used    11661
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      3.1
_cell_volume                     8389(4)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41581
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.074
_exptl_absorpt_coefficient_mu    2.350
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       Block
_exptl_crystal_F_000             4312
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         7366
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0201P)^2^+63.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6799
_reflns_number_total             7366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00827d2.cif
_cod_data_source_block           Co2Ho2
_cod_database_code               7247820
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.549
_shelx_estimated_absorpt_t_min   0.418
_olex2_refinement_description
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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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O33-H33
 0.87 with sigma of 0.01
 Co1-H33
 2.803457 with sigma of 0.02
 C44-H33
 1.910224 with sigma of 0.02
 N1-O5 \\sim N1A-O5A
 with sigma of 0.02
 N1-O1 \\sim N1A-O1A
 with sigma of 0.02
 N1-O4 \\sim N1A-O4A
 with sigma of 0.02
 O1-O5 \\sim O1A-O5A
 with sigma of 0.04
 O1-O4 \\sim O1A-O4A
 with sigma of 0.04
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N1A \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O4A \\sim O4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O5 \\sim O5A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O1 \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O4A, O5A, O1A, N1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, O4, O5, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4A)=Sof(N1A)=Sof(O5A)=Sof(O1A)=1-FVAR(1)
 Sof(N1)=Sof(O1)=Sof(O4)=Sof(O5)=FVAR(1)
 Fixed Sof: H62A(0.5) H62B(0.5) H62C(0.5)
6.a Rotating group:
 O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C44(H44A,H44B)
6.c Me refined with riding coordinates:
 C52(H52A,H52B,H52C), C25(H25A,H25B,H25C), C45(H45A,H45B,H45C), C62(H62A,H62B,
 H62C)
6.d Aromatic/amide H refined with riding coordinates:
 C33(H33A), C13(H13A), C12(H12), C42(H42), C17(H17), C41(H41), C14(H14),
 C37(H37), C19(H19), C39(H39), C20(H20), C40(H40), C34(H34), C22(H22), C21(H21),
  C32(H32)
6.e Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C1(H1A,H1B,H1C)
6.f Idealised tetrahedral OH refined as rotating group:
 O13(H13), O3S(H3S), O2S(H2S), O4S(H4S), O6(H6)
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_shelx_res_checksum              40466
_olex2_submission_special_instructions 'No special instructions were received'