#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:32:20 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179534 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/03/4500350.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4500350
loop_
_publ_author_name
'Liu, Jian-Qiang'
'Huang, Yun-Sheng'
'Zhao, Ying-Yong'
'Jia, Zhen-Bin'
_publ_section_title
;
 Molecular Tectonics of Entangled Metal−Organic Frameworks Based on
 Different Conformational Carboxylates Mixed with a Flexible
 N,N′-Type Ligand
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              569
_journal_paper_doi               10.1021/cg101461w
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C16 H17 Co N2 O4, H2 O'
_chemical_formula_sum            'C16 H19 Co N2 O5'
_chemical_formula_weight         378.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.6540(10)
_cell_angle_beta                 103.8780(10)
_cell_angle_gamma                111.9100(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4306(4)
_cell_length_b                   10.8660(5)
_cell_length_c                   10.9357(5)
_cell_measurement_reflns_used    3030
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.02
_cell_volume                     859.41(7)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7004
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.01
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.9044
_exptl_absorpt_correction_T_min  0.7692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3030
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0264
_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/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                2702
_reflns_number_total             3030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101461w_si_001.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               4500350
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C9 C 0.3875(4) 0.9503(2) 0.5692(3) 0.0587(6) Uani 1 1 d .
H9 H 0.3122 0.9180 0.6173 0.070 Uiso 1 1 calc R
C10 C 0.4732(4) 0.9168(2) 0.3793(3) 0.0596(6) Uani 1 1 d .
H10 H 0.4562 0.8612 0.2972 0.071 Uiso 1 1 calc R
O4 O 0.7412(2) 0.69139(13) 0.53408(14) 0.0467(4) Uani 1 1 d .
Co1 Co 0.43959(3) 0.49473(2) 0.61184(2) 0.02986(11) Uani 1 1 d .
O1 O 0.2872(2) 0.58641(14) 0.53259(14) 0.0451(4) Uani 1 1 d .
O2 O 0.3838(2) 0.59253(14) 0.36096(15) 0.0463(4) Uani 1 1 d .
C6 C 0.2981(3) 0.62202(18) 0.4310(2) 0.0362(4) Uani 1 1 d .
O3 O 0.64659(19) 0.68798(13) 0.70696(14) 0.0431(3) Uani 1 1 d .
N1 N 0.32952(19) 0.43742(15) 0.75119(15) 0.0317(3) Uani 1 1 d .
N2 N 0.2442(2) 0.42688(17) 0.92465(16) 0.0360(4) Uani 1 1 d .
C16 C 0.2429(3) 0.3000(2) 0.7448(2) 0.0400(5) Uani 1 1 d .
H16 H 0.2238 0.2241 0.6777 0.048 Uiso 1 1 calc R
C1 C 0.1905(3) 0.2930(2) 0.8507(2) 0.0438(5) Uani 1 1 d .
H1 H 0.1293 0.2123 0.8703 0.053 Uiso 1 1 calc R
C11 C 0.7459(3) 0.74663(18) 0.64720(18) 0.0349(4) Uani 1 1 d .
C12 C 0.8829(3) 0.8983(2) 0.7131(2) 0.0522(6) Uani 1 1 d .
H12A H 0.9900 0.9125 0.6883 0.063 Uiso 1 1 calc R
H12B H 0.8311 0.9557 0.6779 0.063 Uiso 1 1 calc R
C13 C 0.9416(3) 0.94856(18) 0.8611(2) 0.0424(5) Uani 1 1 d .
C14 C 1.0960(3) 0.9475(2) 0.9391(2) 0.0504(5) Uani 1 1 d .
H14 H 1.1623 0.9120 0.8993 0.061 Uiso 1 1 calc R
C7 C 0.2111(3) 0.7164(2) 0.3954(2) 0.0479(5) Uani 1 1 d .
H7A H 0.1565 0.6906 0.3001 0.057 Uiso 1 1 calc R
H7B H 0.1169 0.7074 0.4342 0.057 Uiso 1 1 calc R
C8 C 0.3573(3) 0.8643(2) 0.4480(2) 0.0458(5) Uani 1 1 d .
C2 C 0.3282(2) 0.51178(19) 0.86107(18) 0.0314(4) Uani 1 1 d .
C4 C 0.2142(3) 0.4642(3) 1.0505(2) 0.0464(5) Uani 1 1 d .
H4A H 0.2995 0.5600 1.1001 0.056 Uiso 1 1 calc R
H4B H 0.2379 0.4054 1.1022 0.056 Uiso 1 1 calc R
C3 C 0.4085(3) 0.6675(2) 0.9091(2) 0.0466(5) Uani 1 1 d .
H3C H 0.4867 0.7057 0.8613 0.070 Uiso 1 1 calc R
H3D H 0.4776 0.7000 1.0018 0.070 Uiso 1 1 calc R
H3E H 0.3128 0.6964 0.8950 0.070 Uiso 1 1 calc R
C5 C 0.0213(3) 0.4477(2) 1.0303(2) 0.0434(5) Uani 1 1 d .
H5A H 0.0027 0.4579 1.1151 0.052 Uiso 1 1 calc R
H5B H -0.0636 0.3543 0.9733 0.052 Uiso 1 1 calc R
O5 O 0.9158(3) 0.3327(3) 0.3180(2) 0.0998(8) Uani 1 1 d D
C15 C 0.8461(3) 1.0015(2) 0.9242(2) 0.0513(5) Uani 1 1 d .
H15 H 0.7412 1.0029 0.8738 0.062 Uiso 1 1 calc R
H5WA H 1.016(2) 0.347(3) 0.375(2) 0.077 Uiso 1 1 d D
H5WB H 0.861(3) 0.369(3) 0.360(2) 0.077 Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C8 C9 C10 121.4(2) . 2_676
C8 C9 H9 119.3 . .
C10 C9 H9 119.3 2_676 .
C9 C10 C8 121.2(2) 2_676 .
C9 C10 H10 119.4 2_676 .
C8 C10 H10 119.4 . .
C11 O4 Co1 132.83(13) . 2_666
O3 Co1 O1 88.13(6) . .
O3 Co1 O2 90.86(6) . 2_666
O1 Co1 O2 161.54(6) . 2_666
O3 Co1 N1 105.20(6) . .
O1 Co1 N1 101.19(6) . .
O2 Co1 N1 96.87(6) 2_666 .
O3 Co1 O4 161.75(6) . 2_666
O1 Co1 O4 88.84(6) . 2_666
O2 Co1 O4 86.37(6) 2_666 2_666
N1 Co1 O4 93.04(6) . 2_666
O3 Co1 Co1 87.07(4) . 2_666
O1 Co1 Co1 84.81(4) . 2_666
O2 Co1 Co1 76.73(4) 2_666 2_666
N1 Co1 Co1 166.38(4) . 2_666
O4 Co1 Co1 74.73(4) 2_666 2_666
C6 O1 Co1 121.28(13) . .
C6 O2 Co1 131.68(14) . 2_666
O2 C6 O1 124.99(18) . .
O2 C6 C7 117.25(19) . .
O1 C6 C7 117.62(18) . .
C11 O3 Co1 119.45(12) . .
C2 N1 C16 106.47(15) . .
C2 N1 Co1 131.71(12) . .
C16 N1 Co1 121.77(12) . .
C2 N2 C1 107.24(16) . .
C2 N2 C4 128.72(17) . .
C1 N2 C4 124.03(17) . .
C1 C16 N1 109.11(18) . .
C1 C16 H16 125.4 . .
N1 C16 H16 125.4 . .
C16 C1 N2 107.05(17) . .
C16 C1 H1 126.5 . .
N2 C1 H1 126.5 . .
O3 C11 O4 125.36(17) . .
O3 C11 C12 118.64(17) . .
O4 C11 C12 115.99(17) . .
C13 C12 C11 115.96(17) . .
C13 C12 H12A 108.3 . .
C11 C12 H12A 108.3 . .
C13 C12 H12B 108.3 . .
C11 C12 H12B 108.3 . .
H12A C12 H12B 107.4 . .
C14 C13 C15 117.71(19) . .
C14 C13 C12 121.0(2) . .
C15 C13 C12 121.3(2) . .
C13 C14 C15 121.0(2) . 2_777
C13 C14 H14 119.5 . .
C15 C14 H14 119.5 2_777 .
C8 C7 C6 108.07(16) . .
C8 C7 H7A 110.1 . .
C6 C7 H7A 110.1 . .
C8 C7 H7B 110.1 . .
C6 C7 H7B 110.1 . .
H7A C7 H7B 108.4 . .
C9 C8 C10 117.4(2) . .
C9 C8 C7 121.2(2) . .
C10 C8 C7 121.3(2) . .
N1 C2 N2 110.14(16) . .
N1 C2 C3 125.31(17) . .
N2 C2 C3 124.55(17) . .
N2 C4 C5 112.29(17) . .
N2 C4 H4A 109.1 . .
C5 C4 H4A 109.1 . .
N2 C4 H4B 109.1 . .
C5 C4 H4B 109.1 . .
H4A C4 H4B 107.9 . .
C2 C3 H3C 109.5 . .
C2 C3 H3D 109.5 . .
H3C C3 H3D 109.5 . .
C2 C3 H3E 109.5 . .
H3C C3 H3E 109.5 . .
H3D C3 H3E 109.5 . .
C4 C5 C5 113.8(2) . 2_567
C4 C5 H5A 108.8 . .
C5 C5 H5A 108.8 2_567 .
C4 C5 H5B 108.8 . .
C5 C5 H5B 108.8 2_567 .
H5A C5 H5B 107.7 . .
H5WA O5 H5WB 108(2) . .
C13 C15 C14 121.3(2) . 2_777
C13 C15 H15 119.4 . .
C14 C15 H15 119.4 2_777 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C9 C8 1.377(3) .
C9 C10 1.378(4) 2_676
C9 H9 0.9300 .
C10 C9 1.378(4) 2_676
C10 C8 1.392(3) .
C10 H10 0.9300 .
O4 C11 1.256(2) .
O4 Co1 2.0735(13) 2_666
Co1 O3 2.0307(13) .
Co1 O1 2.0337(14) .
Co1 O2 2.0371(14) 2_666
Co1 N1 2.0418(15) .
Co1 O4 2.0735(13) 2_666
Co1 Co1 2.8716(5) 2_666
O1 C6 1.255(2) .
O2 C6 1.248(2) .
O2 Co1 2.0371(14) 2_666
C6 C7 1.520(3) .
O3 C11 1.246(2) .
N1 C2 1.323(2) .
N1 C16 1.375(2) .
N2 C2 1.350(2) .
N2 C1 1.369(3) .
N2 C4 1.469(3) .
C16 C1 1.340(3) .
C16 H16 0.9300 .
C1 H1 0.9300 .
C11 C12 1.520(3) .
C12 C13 1.500(3) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.380(3) .
C13 C15 1.386(3) .
C14 C15 1.387(3) 2_777
C14 H14 0.9300 .
C7 C8 1.508(3) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C2 C3 1.497(3) .
C4 C5 1.524(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C3 H3C 0.9600 .
C3 H3D 0.9600 .
C3 H3E 0.9600 .
C5 C5 1.526(4) 2_567
C5 H5A 0.9700 .
C5 H5B 0.9700 .
O5 H5WA 0.856(10) .
O5 H5WB 0.87(3) .
C15 C14 1.387(3) 2_777
C15 H15 0.9300 .
