A multifunctional magnetic material based on a solid solution of Fe(ii)/Co(ii) complexes with a macrocyclic cyclam-based ligand.
Drahoš, Bohuslav; Šalitroš, Ivan; Císařová, Ivana; Herchel, Radovan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11147–11157; doi:10.1039/d1dt01534f

data_7707802
_publ_section_title
;
 A multifunctional magnetic material based on a solid solution of
 Fe(ii)/Co(ii) complexes with a macrocyclic cyclam-based ligand.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11147
_journal_page_last               11157
_journal_paper_doi               10.1039/d1dt01534f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C22 H34 Fe N6, 2(Cl O4), H2 O'
_chemical_formula_sum            'C22 H36 Cl2 Fe N6 O9'
_chemical_formula_weight         655.32
_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_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-22 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.004(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8497(14)
_cell_length_b                   14.052(2)
_cell_length_c                   19.649(3)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      24.5621
_cell_measurement_theta_min      2.3129
_cell_volume                     2719.6(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.10'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'XM, VERSION 2013/2'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.598
_diffrn_reflns_theta_max         24.598
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0041(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4499
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+16.4584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4150
_reflns_number_total             4499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01534f2.cif
_cod_data_source_block           01
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7707802--7707805.cif.
;
_cod_original_cell_volume        2719.5(7)
_cod_database_code               7707802
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.792
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.504(2)
 0.496(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
3. Restrained distances
 O9-H9D
 0.96 with sigma of 0.001
 Cl2-O5 \\sim Cl2A-O5A
 with sigma of 0.02
 Cl2-O6 \\sim Cl2A-O6A
 with sigma of 0.02
 Cl2-O8 \\sim Cl2A-O8A
 with sigma of 0.02
 Cl2-O7 \\sim Cl2A-O7A
 with sigma of 0.02
 O6-O7 \\sim O6A-O7A
 with sigma of 0.04
 O8-O7 \\sim O8A-O7A
 with sigma of 0.04
 O5-O7 \\sim O5A-O7A
 with sigma of 0.04
 O6-O8 \\sim O6A-O8A
 with sigma of 0.04
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O5-O8 \\sim O5A-O8A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(O8)
Uanis(O6A) = Uanis(O6) = Uanis(O5A) = Uanis(O5)
5. Rigid body (RIGU) restrains
 Cl2A, O5A, O6A, O8A, O7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O8, O6, O7, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O7A)=Sof(Cl2A)=Sof(O6A)=Sof(O5A)=Sof(O8A)=1-FVAR(1)
 Sof(Cl2)=Sof(O5)=Sof(O6)=Sof(O8)=Sof(O7)=FVAR(1)
7.a Riding coordinates:
 O9(H9C,H9D)
7.b Ternary CH refined with riding coordinates:
 N2(H2), N4(H4)
7.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B), C8(H8A,H8B), C2(H2A,H2B),
 C7(H7A,H7B), C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B), C6(H6A,H6B),
 C17(H17A,H17B)
7.d Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C14(H14), C20(H20), C13(H13), C15(H15), C16(H16), C19(H19)
;
_shelx_res_checksum              95975
_shelx_hkl_checksum              66923
_olex2_submission_special_instructions 'No special instructions were received'