Hexagonal Co6 and zigzag Co4 cluster based magnetic MOFs with a pcu net for selective catalysis
Yao, Ru-Xin; Qiao, Xiao-Hui; Cui, Xin; Jia, Xiao-Xia; Zhang, Xian-Ming; Inorganic Chemistry Frontiers 3 (2016) 78–; doi:10.1039/C5QI00159E

data_4348985
_publ_section_title
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 Hexagonal Co6 and zigzag Co4 cluster based magnetic MOFs with a pcu net
 for selective catalysis
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_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              78
_journal_paper_doi               10.1039/C5QI00159E
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C16 H14 Co2 N4 O8'
_chemical_formula_sum            'C16 H14 Co2 N4 O8'
_chemical_formula_weight         508.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
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_audit_update_record
;
2015-10-06 deposited with the CCDC.
2015-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9765(17)
_cell_length_b                   15.0880(15)
_cell_length_c                   15.9616(16)
_cell_measurement_reflns_used    3756
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.700
_cell_measurement_theta_min      2.253
_cell_volume                     3847.6(7)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22442
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.276
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.702772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
? was used for absorption correction.
R(int) was 0.0490 before and 0.0337 after correction.
The Ratio of minimum to maximum transmission is 0.7028.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4089
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0996P)^2^+7.7106P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3243
_reflns_number_total             4089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00159e2.cif
_cod_data_source_block           2
_cod_database_code               4348985
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.696
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C6' \\sim C7 \\sim C7'
\\sim C8 \\sim C8' \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14
\\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6') \\sim
Ueq, Uanis(C7') \\sim Ueq, Uanis(C8') \\sim Ueq: with sigma of 0.1 and sigma
for terminal atoms of 0.2
3. Others
 Sof(C6')=Sof(H6'A)=Sof(H6'B)=Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(C8')=Sof(H8'A)=
 Sof(H8'B)=Sof(H8'C)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=FVAR(1)
 Fixed Sof: H12A(0.5) H12B(0.5) H13A(0.5) H13B(0.5) H14B(0.5) H14C(0.5)
 H18A(0.5) H18B(0.5) H19A(0.5) H19B(0.5) H20B(0.5) H20C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C6'(H6'A,H6'B), C7(H7A,H7B), C7'(H7'A,H7'B), C12(H12A,H12B),
 C13(H13A,H13B), C18(H18A,H18B), C19(H19A,H19B)
4.b Me refined with riding coordinates:
 C8'(H8'A,H8'B,H8'C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
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