Switching a 2D Co(II) layer to a 3D Co7-cluster-based metal-organic framework: syntheses, crystal structures, and magnetic properties.
Chen, Di-Ming; Ma, Xiao-Zhou; Zhang, Xue-Jing; Xu, Na; Cheng, Peng; Inorganic chemistry 54 (2015) 2976–2982; doi:10.1021/acs.inorgchem.5b00074

data_4346032
_publ_section_title
;
 Switching a 2D Co(II) layer to a 3D Co7-cluster-based metal-organic
 framework: syntheses, crystal structures, and magnetic properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2976
_journal_page_last               2982
_journal_paper_doi               10.1021/acs.inorgchem.5b00074
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'0.5(C120 H100 Co14 N36 O40), 2(C10 H6 N3 O2)'
_chemical_formula_sum            'C89 H105 Co7 N27 O32'
_chemical_formula_weight         2477.51
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.975(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.4430(7)
_cell_length_b                   22.1987(13)
_cell_length_c                   17.7628(12)
_cell_measurement_temperature    293(2)
_cell_volume                     5526.5(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28118
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.098
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2246
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         2.670
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9718
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+2.7505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1818
_reflns_number_gt                7646
_reflns_number_total             9718
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00074_si_002.cif
_cod_data_source_block           3
_cod_database_code               4346032
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H14(0.031) H21(0.027) H23(0.029) H31(0.037) H32(0.034) H33(0.028)
 H35A(0.032) H35B(0.032) H36(0.029) H37(0.028) H38A(0.034) H38B(0.034)
 H39(0.027) H41(0.041) H42(0.038) H43(0.033) H44(0.037) H45(0.028) H46(0.034)
 H47(0.049) H50A(0.031) H50B(0.031) H51(0.041) H53(0.055) H61(0.07) H65(0.076)
 H67(0.074) H75A(0.069) H75B(0.069) H77(0.085) H86(0.07) H87(0.068) H2AA(0.055)
 H2AB(0.055) H1AA(0.071) H1AB(0.071)
 Fixed X: Co1(0.5) H14(0.215) H21(0.7152) H23(0.5648) H31(0.8026) H32(0.6112)
 H33(0.2242) H35A(0.3808) H35B(0.3512) H36(0.8304) H37(0.6621) H38A(1.1368)
 H38B(1.1493) H39(0.7759) H41(0.9581) H42(-0.1099) H43(0.0854) H44(0.4616)
 H45(0.7237) H46(-0.0741) H47(1.0255) H50A(-0.2192) H50B(-0.2226) H51(0.048)
 H53(0.869) H61(0.1822) H65(-0.0318) H67(-0.0753) H75A(0.2709) H75B(0.2466)
 H77(-0.1883) H86(0.1074) H87(0.0418) H2AA(0.519) H2AB(0.4172) H1AA(0.5361)
 H1AB(0.5021)
 Fixed Y: Co1(0) H14(0.1104) H21(0.3283) H23(0.3032) H31(0.1993) H32(0.3365)
 H33(-0.0651) H35A(0.3125) H35B(0.2932) H36(0.4008) H37(0.166) H38A(0.2215)
 H38B(0.2544) H39(0.321) H41(0.2244) H42(-0.0561) H43(0.0955) H44(0.3078)
 H45(0.1819) H46(0.0905) H47(0.2371) H50A(-0.0261) H50B(0.0436) H51(-0.053)
 H53(0.2119) H61(0.0414) H65(-0.1082) H67(0.0774) H75A(-0.0319) H75B(-0.1006)
 H77(-0.0723) H86(-0.1314) H87(0.0662) H2AA(0.1135) H2AB(0.1191) H1AA(0.027)
 H1AB(0.0988)
 Fixed Z: Co1(0.5) H14(0.6369) H21(0.6238) H23(0.5495) H31(0.8088) H32(0.8135)
 H33(0.6696) H35A(0.5436) H35B(0.6198) H36(0.6967) H37(0.7493) H38A(0.8561)
 H38B(0.7806) H39(0.8792) H41(0.871) H42(0.5911) H43(0.7175) H44(0.7395)
 H45(0.5477) H46(0.7231) H47(0.6674) H50A(0.6865) H50B(0.698) H51(0.5843)
 H53(0.6046) H61(0.0844) H65(0.0987) H67(0.1771) H75A(0.0215) H75B(0.0246)
 H77(0.0889) H86(0.0669) H87(0.1109) H2AA(0.7945) H2AB(0.7833) H1AA(0.1624)
 H1AB(0.1615)
;
_olex2_submission_special_instructions 'No special instructions were received'