In Situ Generation of NiO Nanoparticles in a Magnetic Metal-Organic Framework Exhibiting Three-Dimensional Magnetic Ordering.
Meng, Xixi; Zhang, Xuejing; Bing, Yanmin; Xu, Na; Shi, Wei; Cheng, Peng; Inorganic chemistry 55 (2016) 12938–12943; doi:10.1021/acs.inorgchem.6b02376

data_4349318
_publ_section_title
;
 In Situ Generation of NiO Nanoparticles in a Magnetic Metal-Organic
 Framework Exhibiting Three-Dimensional Magnetic Ordering.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12938
_journal_page_last               12943
_journal_paper_doi               10.1021/acs.inorgchem.6b02376
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '0.5(C56 H40 N4 Ni6 O28)'
_chemical_formula_sum            'C28 H20 N2 Ni3 O14'
_chemical_formula_weight         784.59
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.951(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9394(5)
_cell_length_b                   17.2285(8)
_cell_length_c                   7.6644(4)
_cell_measurement_reflns_used    3166
_cell_measurement_temperature    128.40(14)
_cell_measurement_theta_max      29.1349
_cell_measurement_theta_min      2.3596
_cell_volume                     1388.89(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      128.40(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0559971000
_diffrn_orient_matrix_UB_12      0.0220312000
_diffrn_orient_matrix_UB_13      0.0076028000
_diffrn_orient_matrix_UB_21      0.0349956000
_diffrn_orient_matrix_UB_22      -0.0263644000
_diffrn_orient_matrix_UB_23      0.0661066000
_diffrn_orient_matrix_UB_31      0.0137658000
_diffrn_orient_matrix_UB_32      -0.0226102000
_diffrn_orient_matrix_UB_33      -0.0696106000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5098
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97016
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+2.0210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                2180
_reflns_number_total             2442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02376_si_002.cif
_cod_data_source_block           p120611d
_cod_database_code               4349318
_chemical_oxdiff_formula         C12Ni1
_chemical_oxdiff_usercomment     Ni-DMF
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H5Aa-H5Aa_$1
 2.1 with sigma of 0.02
 H5Aa-H5Aa_$1
 2.1 with sigma of 0.02
 H5Aa-H5Aa_$1
 2.2 with sigma of 0.02
 H5Aa-H5Aa_$1
 2.3 with sigma of 0.01
3.a Riding coordinates:
 O5AA(H5Aa,H5Ab)
3.b Aromatic/amide H refined with riding coordinates:
 C7AA(H7AA), C8AA(H8AA), C0AA(H0AA), C6AA(H6AA), C4AA(H4AA), C3BA(H3BA),
 C4BA(H4BA), C2AA(H2AA)
;
_olex2_submission_special_instructions 'No special instructions were received'