Metallocyclic Ni4Ln2M2 single-molecule magnets
Liu, Mei-Jiao; Hu, kong-Qiu; Liu, Cai-Ming; Cui, Ai-Li; Kou, Hui-Zhong; Dalton Trans.  (2017) –; doi:10.1039/C7DT00948H

data_7042775
_publ_section_title
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 Metallocyclic Ni4Ln2M2 single-molecule magnets
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_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00948H
_journal_year                    2017
_chemical_formula_moiety
'C96 H100 Cr2 Gd2 N20 Ni4 O18, 3(C3 H7 N O), 13(O), 2(C2 H3 N)'
_chemical_formula_sum            'C109 H153 Cr2 Gd2 N25 Ni4 O34'
_chemical_formula_weight         3010.89
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-13 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7191(8)
_cell_length_b                   22.6110(9)
_cell_length_c                   19.4149(8)
_cell_measurement_reflns_used    34824
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.3889
_cell_measurement_theta_min      2.0626
_cell_volume                     7057.5(5)
_computing_cell_refinement       'SAINT, V8.34A'
_computing_data_collection       'SAINT, V8.34A'
_computing_data_reduction        'SAINT, V8.34A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.1
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34314
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         2.985
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6520
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.401
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         12752
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0836P)^2^+34.7796P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7765
_reflns_number_total             12752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00948h2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7042775
_shelxl_version_number           2013-2
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C53-O11
 1.25 with sigma of 0.01
 C53-N12
 1.3 with sigma of 0.01
 N12-C52 = N12-C54
 1.45 with sigma of 0.01
 O11-N12
 2.26 with sigma of 0.01
 C53-C54 = C53-C52
 2.4 with sigma of 0.01
 C52-C54
 2.48 with sigma of 0.01
3. Restrained planarity
 C52, O11, N12, C54, C53
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) O11(0.5) N12(0.5) C54(0.5)
 H54A(0.5) H54B(0.5) H54C(0.5) C53(0.5) H53(0.5) O8W(0.5) O9W(0.5) O7W(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C43(H43A,H43B), C44(H44A,H44B)
6.c Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
6.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15), C17(H17), C19(H19), C28(H28),
 C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39), C40(H40),
  C48(H48), C51(H51), C53(H53)
6.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C56(H56A,H56B,H56C)
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_olex2_submission_special_instructions 'No special instructions were received'