Octanuclear Heterobimetallic {Ni4Ln4} Assemblies Possessing Ln4 Square Grid [2 ×2] Motifs: Synthesis, Structure, and Magnetism.
Biswas, Sourav; Goura, Joydeb; Das, Sourav; Topping, Craig V.; Brambleby, Jamie; Goddard, Paul A.; Chandrasekhar, Vadapalli; Inorganic chemistry 55 (2016) 8422–8436; doi:10.1021/acs.inorgchem.6b01019

data_4348149
_publ_section_title
;
 Octanuclear Heterobimetallic {Ni4Ln4} Assemblies Possessing Ln4 Square
 Grid [2 \\times 2] Motifs: Synthesis, Structure, and Magnetism.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8422
_journal_page_last               8436
_journal_paper_doi               10.1021/acs.inorgchem.6b01019
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C88 H108 Gd4 N12 Ni4 O24, 19.3333(O), 4(Cl), 4(C O)'
_chemical_formula_sum            'C92 H108 Cl4 Gd4 N12 Ni4 O47.33333'
_chemical_formula_weight         3144.87
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   34.090(5)
_cell_length_b                   34.090(5)
_cell_length_c                   34.090(5)
_cell_measurement_reflns_used    9633
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.24
_cell_volume                     39617(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            177303
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         4.141
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.699
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5394
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.7233.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             18704
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 2482 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5822
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+111.1776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5411
_reflns_number_total             5822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01019_si_002.cif
_cod_data_source_block           Complex3
_cod_depositor_comments
;

2021-04-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C276 H324 Cl12 Gd12 N36 Ni12 O142'
_cod_original_formula_weight         9434.61
_cod_original_formula_moiety
'3(C88 H108 Gd4 N12 Ni4 O24), 58(O), 12(Cl), 12(C O)'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        39617(17)
_cod_database_code               4348149
_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
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O31-C0AA
 1.5 with sigma of 0.02
 C8-H1
 1.89395 with sigma of 0.02
 C22-H4
 1.893627 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C0AA) \\sim Ueq, Uanis(O31) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.05
Uanis(Cl2) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(O1AA) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C22(H22A,H22B), C10(H10A,H10B),
 C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C7(H7), C9(H9), C3(H3), C16(H16), C19(H19)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              13337
_shelx_hkl_checksum              51272
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'