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_7247821
_publ_section_title
;
 Ferromagnetically coupled CoII2LnIII2 complexes (where LnIII = Ho, Er,
 Yb): experimental and theoretical investigations
;
_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 N4 O20 Yb2, 8(C H4 O), 3(N O3)'
_chemical_formula_sum            'C74 H101 Co2 N7 O37 Yb2'
_chemical_formula_weight         2144.55
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.03.08 svn.r54f81f84 for OlexSys, GUI svn.r6487)
;
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.400(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.7585(7)
_cell_length_b                   16.0409(5)
_cell_length_c                   19.8206(6)
_cell_measurement_reflns_used    15117
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4050
_cell_measurement_theta_min      1.8460
_cell_volume                     8454.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.856
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Red Orange'
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       Block
_exptl_crystal_F_000             4336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         7455
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0301P)^2^+23.5288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6042
_reflns_number_total             7455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00827d2.cif
_cod_data_source_block           Co2Yb2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '100 (2)' was changed
to '100(2)' -- the value was reformatted.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7247821
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
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
 0.85 with sigma of 0.01
 O13-H13
 0.85 with sigma of 0.01
 C44-H33
 1.887058 with sigma of 0.02
 C24-H13
 1.90588 with sigma of 0.02
 O1-N2 \\sim O1A-N2A
 with sigma of 0.02
 N2-O2 \\sim N2A-O2A
 with sigma of 0.02
 N2-O4 \\sim N2A-O4A
 with sigma of 0.02
 O4-O2 \\sim O4A-O2A
 with sigma of 0.04
 O1-O4 \\sim O1A-O4A
 with sigma of 0.04
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2A \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O1A \\sim O1: 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
4. Rigid body (RIGU) restrains
 O2A, N2A, O1A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, O4, O2, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O2A)=Sof(O4A)=Sof(N2A)=Sof(O1A)=1-FVAR(1)
 Sof(O1)=Sof(N2)=Sof(O4)=Sof(O2)=FVAR(1)
 Fixed Sof: H52A(0.5) H52B(0.5) H52C(0.5)
6.a Rotating group:
 O3W(H3WA,H3WB)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C17(H17), C32(H32), C39(H39), C19(H19), C12(H12), C13(H13A),
 C14(H14), C34(H34), C22(H22), C33(H33A), C40(H40), C41(H41), C42(H42),
 C21(H21), C20(H20)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C52(H52A,H52B,H52C), C72(H72A,H72B,H72C), C2S(H2SA,H2SB,
 H2SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C45(H45A,H45B,H45C), C1S(H1SA,
 H1SB,H1SC)
6.e Idealised tetrahedral OH refined as rotating group:
 O2S(H2S), O3S(H3S), O4S(H4S), O1S(H1S)
;
_shelx_res_checksum              22987
_olex2_submission_special_instructions 'No special instructions were received'