#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/66/4506619.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_4506619
loop_
_publ_author_name
'Cui, Jiehu'
'Li, Yizhi'
'Guo, Zijian'
'Zheng, Hegen'
_publ_section_title
;
 Six New Co-Coordination Polymers Based on a Tripodal Carboxylate
 Ligand
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3610
_journal_paper_doi               10.1021/cg3004323
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C54 H42 Co3 N2 O22'
_chemical_formula_sum            'C54 H42 Co3 N2 O22'
_chemical_formula_weight         1247.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.758(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.403(3)
_cell_length_b                   10.834(2)
_cell_length_c                   17.981(3)
_cell_measurement_reflns_used    5296
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      2.27
_cell_volume                     3027.2(9)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SMART (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'phi and omega scans'
_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  0.1031
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15883
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5296
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0708
_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/[σ²(Fo²)+(0.0856P)²+10.3212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.1963
_reflns_number_gt                4474
_reflns_number_total             5296
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4506307
_cod_data_source_file            cg3004323_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        3027.0(10)
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4506619
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
C1 C 1.0292(3) 0.0265(5) 0.2717(3) 0.0252(11) Uani 1 1 d U
C2 C 0.9711(3) 0.0183(5) 0.3139(3) 0.0273(12) Uani 1 1 d U
C3 C 0.9473(4) -0.0963(6) 0.3296(4) 0.0350(13) Uani 1 1 d U
H3A H 0.9695 -0.1696 0.3163 0.042 Uiso 1 1 d R
C4 C 0.8915(4) -0.1053(6) 0.3646(4) 0.0439(15) Uani 1 1 d U
C5 C 0.8576(4) -0.0007(6) 0.3839(4) 0.0443(16) Uani 1 1 d U
H5A H 0.8184 -0.0073 0.4079 0.053 Uiso 1 1 d R
C6 C 0.8831(4) 0.1126(6) 0.3684(4) 0.0444(16) Uani 1 1 d U
C7 C 0.9398(4) 0.1235(6) 0.3338(4) 0.0368(14) Uani 1 1 d U
H7A H 0.9572 0.2037 0.3242 0.044 Uiso 1 1 d R
C8 C 0.8191(5) -0.2495(7) 0.4138(5) 0.0528(18) Uani 1 1 d U
C9 C 0.8507(5) -0.2339(7) 0.4973(5) 0.0555(19) Uani 1 1 d U
H9A H 0.9034 -0.1949 0.5274 0.067 Uiso 1 1 calc R
C10 C 0.8036(4) -0.2767(6) 0.5378(4) 0.0412(15) Uani 1 1 d U
H10A H 0.8259 -0.2676 0.5970 0.049 Uiso 1 1 d R
C11 C 0.7258(4) -0.3336(5) 0.4925(4) 0.0311(12) Uani 1 1 d U
C12 C 0.6936(4) -0.3467(7) 0.4076(4) 0.0471(16) Uani 1 1 d U
H12A H 0.6387 -0.3853 0.3759 0.057 Uiso 1 1 d R
C13 C 0.7417(5) -0.3033(8) 0.3689(5) 0.057(2) Uani 1 1 d U
H13A H 0.7198 -0.3114 0.3097 0.069 Uiso 1 1 d R
C14 C 0.6742(3) -0.3847(5) 0.5346(3) 0.0263(11) Uani 1 1 d U
C15 C 0.7971(5) 0.2290(7) 0.4174(5) 0.0543(19) Uani 1 1 d U
C16 C 0.8266(5) 0.2021(8) 0.5009(5) 0.062(2) Uani 1 1 d U
H16A H 0.8834 0.1690 0.5325 0.075 Uiso 1 1 d R
C17 C 0.7741(4) 0.2238(7) 0.5379(4) 0.0472(16) Uani 1 1 d U
H17A H 0.7936 0.2032 0.5955 0.057 Uiso 1 1 d R
C18 C 0.6932(4) 0.2727(5) 0.4929(4) 0.0328(13) Uani 1 1 d U
C19 C 0.6641(4) 0.2971(6) 0.4088(4) 0.0438(15) Uani 1 1 d U
H19A H 0.6070 0.3286 0.3766 0.053 Uiso 1 1 d R
C20 C 0.7169(5) 0.2759(7) 0.3716(5) 0.058(2) Uani 1 1 d U
H20A H 0.6976 0.2943 0.3137 0.069 Uiso 1 1 d R
C21 C 0.6357(3) 0.3018(5) 0.5343(3) 0.0259(11) Uani 1 1 d U
C22 C 1.2525(4) 0.0561(6) 0.3444(4) 0.0390(14) Uani 1 1 d U
H22A H 1.2042 0.0188 0.3441 0.047 Uiso 1 1 calc R
C23 C 1.3310(4) 0.0280(6) 0.4083(4) 0.0392(14) Uani 1 1 d U
H23A H 1.3352 -0.0256 0.4525 0.047 Uiso 1 1 d R
C24 C 1.4038(3) 0.0770(5) 0.4088(3) 0.0304(12) Uani 1 1 d U
C25 C 1.3933(4) 0.1611(5) 0.3475(4) 0.0350(13) Uani 1 1 d U
H25A H 1.4423 0.2020 0.3475 0.042 Uiso 1 1 d R
C26 C 1.3112(4) 0.1843(6) 0.2856(4) 0.0352(13) Uani 1 1 d U
H26A H 1.3052 0.2391 0.2435 0.042 Uiso 1 1 calc R
C27 C 1.4908(4) 0.0441(6) 0.4712(4) 0.0376(13) Uani 1 1 d U
Co1 Co 1.11684(4) 0.18883(6) 0.19316(4) 0.0222(2) Uani 1 1 d U
Co2 Co 1.0000 0.0000 0.0000 0.0202(3) Uani 1 2 d SU
H11A H 1.0967(18) 0.391(8) 0.237(4) 0.08(3) Uiso 1 1 d D
H11B H 1.182(2) 0.383(6) 0.2973(15) 0.034(17) Uiso 1 1 d D
N1 N 1.2403(3) 0.1332(4) 0.2825(3) 0.0300(10) Uani 1 1 d U
O1 O 1.0563(2) 0.1314(3) 0.2654(2) 0.0315(9) Uani 1 1 d U
O2 O 1.0444(3) -0.0718(4) 0.2453(3) 0.0438(11) Uani 1 1 d U
O3 O 0.8691(4) -0.2216(5) 0.3735(4) 0.0761(18) Uani 1 1 d U
O4 O 0.5941(2) -0.3958(4) 0.4879(2) 0.0322(9) Uani 1 1 d U
O5 O 0.7115(2) -0.4134(4) 0.6091(2) 0.0342(9) Uani 1 1 d U
O6 O 0.8519(4) 0.2226(5) 0.3802(4) 0.0787(18) Uani 1 1 d U
O7 O 0.5635(2) 0.3470(3) 0.4886(2) 0.0300(8) Uani 1 1 d U
O8 O 0.6661(2) 0.2755(4) 0.6099(2) 0.0307(9) Uani 1 1 d U
O9 O 1.0831(2) 0.0085(3) 0.1321(2) 0.0228(8) Uani 1 1 d U
H9B H 1.0595 -0.0333 0.1563 0.027 Uiso 1 1 d R
H9C H 1.1298 -0.0279 0.1412 0.027 Uiso 1 1 d R
O10 O 0.9995(2) 0.2731(4) 0.1166(2) 0.0373(9) Uani 1 1 d U
H10C H 1.0081 0.3343 0.0917 0.045 Uiso 1 1 d R
H10D H 0.9763 0.2996 0.1462 0.045 Uiso 1 1 d R
O11 O 1.1465(3) 0.3639(4) 0.2478(3) 0.0395(10) Uani 1 1 d DU
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'
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'
Co Co 0.3494 0.9721 '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
O2 C1 O1 126.0(4) . .
O2 C1 C2 116.5(5) . .
O1 C1 C2 117.5(5) . .
C7 C2 C3 120.1(5) . .
C7 C2 C1 120.8(5) . .
C3 C2 C1 119.1(5) . .
C2 C3 C4 119.8(6) . .
C2 C3 H3A 120.1 . .
C4 C3 H3A 120.1 . .
O3 C4 C3 114.9(6) . .
O3 C4 C5 123.6(5) . .
C3 C4 C5 121.4(6) . .
C6 C5 C4 117.7(5) . .
C6 C5 H5A 121.1 . .
C4 C5 H5A 121.2 . .
O6 C6 C5 124.1(5) . .
O6 C6 C7 114.1(6) . .
C5 C6 C7 121.7(6) . .
C2 C7 C6 119.3(6) . .
C2 C7 H7A 120.6 . .
C6 C7 H7A 120.1 . .
C13 C8 C9 120.9(6) . .
C13 C8 O3 118.1(7) . .
C9 C8 O3 120.8(7) . .
C8 C9 C10 119.6(6) . .
C8 C9 H9A 120.2 . .
C10 C9 H9A 120.2 . .
C11 C10 C9 119.5(6) . .
C11 C10 H10A 120.2 . .
C9 C10 H10A 120.3 . .
C12 C11 C10 120.4(5) . .
C12 C11 C14 118.7(5) . .
C10 C11 C14 121.0(5) . .
C11 C12 C13 119.0(6) . .
C11 C12 H12A 120.2 . .
C13 C12 H12A 120.8 . .
C8 C13 C12 120.6(7) . .
C8 C13 H13A 119.5 . .
C12 C13 H13A 119.8 . .
O5 C14 O4 125.3(5) . .
O5 C14 C11 119.5(5) . .
O4 C14 C11 115.2(5) . .
C20 C15 C16 121.0(6) . .
C20 C15 O6 117.8(7) . .
C16 C15 O6 120.8(7) . .
C17 C16 C15 119.3(7) . .
C17 C16 H16A 120.6 . .
C15 C16 H16A 120.1 . .
C16 C17 C18 120.6(6) . .
C16 C17 H17A 119.7 . .
C18 C17 H17A 119.7 . .
C17 C18 C19 119.4(5) . .
C17 C18 C21 121.0(5) . .
C19 C18 C21 119.6(5) . .
C20 C19 C18 120.1(6) . .
C20 C19 H19A 120.1 . .
C18 C19 H19A 119.8 . .
C15 C20 C19 119.7(7) . .
C15 C20 H20A 119.9 . .
C19 C20 H20A 120.4 . .
O7 C21 O8 127.7(5) . .
O7 C21 C18 116.5(5) . .
O8 C21 C18 115.8(5) . .
N1 C22 C23 124.5(6) . .
N1 C22 H22A 117.8 . .
C23 C22 H22A 117.8 . .
C24 C23 C22 119.4(6) . .
C24 C23 H23A 120.2 . .
C22 C23 H23A 120.4 . .
C23 C24 C25 117.5(5) . .
C23 C24 C27 123.0(5) . .
C25 C24 C27 119.5(5) . .
C24 C25 C26 118.8(5) . .
C24 C25 H25A 120.4 . .
C26 C25 H25A 120.8 . .
N1 C26 C25 124.1(5) . .
N1 C26 H26A 118.0 . .
C25 C26 H26A 118.0 . .
C27 C27 C24 124.8(7) 3_856 .
O8 Co1 O10 92.40(16) 4_665 .
O8 Co1 O11 94.33(17) 4_665 .
O10 Co1 O11 82.78(17) . .
O8 Co1 O1 171.42(15) 4_665 .
O10 Co1 O1 85.61(16) . .
O11 Co1 O1 93.69(16) . .
O8 Co1 N1 89.60(17) 4_665 .
O10 Co1 N1 169.84(17) . .
O11 Co1 N1 87.14(18) . .
O1 Co1 N1 93.82(17) . .
O8 Co1 O9 84.76(14) 4_665 .
O10 Co1 O9 95.61(15) . .
O11 Co1 O9 178.12(16) . .
O1 Co1 O9 87.12(14) . .
N1 Co1 O9 94.50(16) . .
O7 Co2 O7 180.0(2) 4_665 2_645
O7 Co2 O4 93.25(15) 4_665 2_655
O7 Co2 O4 86.75(15) 2_645 2_655
O7 Co2 O4 86.75(15) 4_665 4_655
O7 Co2 O4 93.25(15) 2_645 4_655
O4 Co2 O4 180.0(2) 2_655 4_655
O7 Co2 O9 92.79(14) 4_665 3_755
O7 Co2 O9 87.21(14) 2_645 3_755
O4 Co2 O9 88.24(14) 2_655 3_755
O4 Co2 O9 91.76(14) 4_655 3_755
O7 Co2 O9 87.21(14) 4_665 .
O7 Co2 O9 92.79(14) 2_645 .
O4 Co2 O9 91.76(14) 2_655 .
O4 Co2 O9 88.24(14) 4_655 .
O9 Co2 O9 180.0 3_755 .
C22 N1 C26 115.6(5) . .
C22 N1 Co1 122.7(4) . .
C26 N1 Co1 121.3(4) . .
C1 O1 Co1 129.6(3) . .
C4 O3 C8 123.0(6) . .
C14 O4 Co2 131.7(3) . 2_645
C6 O6 C15 121.7(6) . .
C21 O7 Co2 132.6(3) . 2_655
C21 O8 Co1 129.4(3) . 4_566
Co2 O9 Co1 119.10(15) . .
Co2 O9 H9B 107.6 . .
Co1 O9 H9B 107.6 . .
Co2 O9 H9C 107.5 . .
Co1 O9 H9C 107.5 . .
H9B O9 H9C 107.0 . .
Co1 O10 H10C 109.6 . .
Co1 O10 H10D 109.5 . .
H10C O10 H10D 108.2 . .
Co1 O11 H11A 101(5) . .
Co1 O11 H11B 129(4) . .
H11A O11 H11B 109.6(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.243(7) .
C1 O1 1.256(7) .
C1 C2 1.516(7) .
C2 C7 1.377(8) .
C2 C3 1.378(8) .
C3 C4 1.376(8) .
C3 H3A 0.9599 .
C4 O3 1.349(8) .
C4 C5 1.392(9) .
C5 C6 1.376(9) .
C5 H5A 0.9599 .
C6 O6 1.365(8) .
C6 C7 1.389(8) .
C7 H7A 0.9599 .
C8 C13 1.352(11) .
C8 C9 1.357(11) .
C8 O3 1.394(7) .
C9 C10 1.399(9) .
C9 H9A 0.9300 .
C10 C11 1.373(8) .
C10 H10A 0.9599 .
C11 C12 1.376(9) .
C11 C14 1.516(7) .
C12 C13 1.389(9) .
C12 H12A 0.9601 .
C13 H13A 0.9601 .
C14 O5 1.236(6) .
C14 O4 1.269(6) .
C15 C20 1.360(11) .
C15 C16 1.381(11) .
C15 O6 1.390(7) .
C16 C17 1.372(9) .
C16 H16A 0.9600 .
C17 C18 1.375(9) .
C17 H17A 0.9600 .
C18 C19 1.386(9) .
C18 C21 1.525(7) .
C19 C20 1.379(9) .
C19 H19A 0.9600 .
C20 H20A 0.9598 .
C21 O7 1.251(7) .
C21 O8 1.249(6) .
C22 N1 1.330(8) .
C22 C23 1.367(8) .
C22 H22A 0.9300 .
C23 C24 1.370(8) .
C23 H23A 0.9601 .
C24 C25 1.377(8) .
C24 C27 1.465(8) .
C25 C26 1.383(8) .
C25 H25A 0.9601 .
C26 N1 1.331(7) .
C26 H26A 0.9300 .
C27 C27 1.338(13) 3_856
Co1 O8 2.069(4) 4_665
Co1 O10 2.090(4) .
Co1 O11 2.090(4) .
Co1 O1 2.100(3) .
Co1 N1 2.110(4) .
Co1 O9 2.187(3) .
Co2 O7 2.053(3) 4_665
Co2 O7 2.053(3) 2_645
Co2 O4 2.080(3) 2_655
Co2 O4 2.080(3) 4_655
Co2 O9 2.156(3) 3_755
Co2 O9 2.156(3) .
O4 Co2 2.080(3) 2_645
O7 Co2 2.053(3) 2_655
O8 Co1 2.069(4) 4_566
O9 H9B 0.8501 .
O9 H9C 0.8501 .
O10 H10C 0.8501 .
O10 H10D 0.8499 .
O11 H11A 0.850(10) .
O11 H11B 0.851(10) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 1.000 337 88 ' '
2 1.000 0.500 0.500 337 88 ' '
