#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/66/4506621.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_4506621
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 H38 Co3 N2 O22'
_chemical_formula_sum            'C54 H38 Co3 N2 O22'
_chemical_formula_weight         1243.65
_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                 116.170(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.4870(19)
_cell_length_b                   10.8823(11)
_cell_length_c                   18.0449(19)
_cell_measurement_reflns_used    7632
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.26
_cell_volume                     3081.9(6)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21619
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1266
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7632
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0486P)²+3.5838P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1290
_reflns_number_gt                5782
_reflns_number_total             7697
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4506309
_cod_data_source_file            cg3004323_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4506621
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 1.03153(18) 0.9748(3) 0.27324(17) 0.0272(6) Uani 1 1 d U
C2 C 0.97303(18) 0.9800(3) 0.31515(17) 0.0284(6) Uani 1 1 d U
C3 C 0.9467(2) 0.8729(3) 0.3387(2) 0.0361(7) Uani 1 1 d U
H3A H 0.9683 0.7945 0.3324 0.043 Uiso 1 1 d R
C4 C 0.8886(2) 0.8813(3) 0.3716(2) 0.0438(8) Uani 1 1 d U
C5 C 0.8579(2) 0.9929(3) 0.3833(2) 0.0432(8) Uani 1 1 d U
H5A H 0.8176 0.9970 0.4061 0.052 Uiso 1 1 d R
C6 C 0.8865(2) 1.0986(3) 0.3602(2) 0.0445(8) Uani 1 1 d U
C7 C 0.9439(2) 1.0933(3) 0.3267(2) 0.0377(7) Uani 1 1 d U
H7A H 0.9642 1.1673 0.3126 0.045 Uiso 1 1 d R
C8 C 0.8064(3) 0.7626(4) 0.4240(3) 0.0591(11) Uani 1 1 d U
H8A H 0.6354 1.3818 0.3745 0.071 Uiso 1 1 d R
C9 C 0.7266(3) 0.7160(4) 0.3771(3) 0.0601(11) Uani 1 1 d U
H9C H 0.7090 0.6977 0.3198 0.072 Uiso 1 1 d R
C10 C 0.6717(2) 0.6961(4) 0.4121(2) 0.0472(9) Uani 1 1 d U
H10C H 0.6174 0.6654 0.3801 0.057 Uiso 1 1 calc R
C11 C 0.69748(19) 0.7216(3) 0.49500(18) 0.0304(6) Uani 1 1 d U
C12 C 0.7776(2) 0.7718(4) 0.5406(2) 0.0441(8) Uani 1 1 d U
C13 C 0.8325(3) 0.7915(4) 0.5055(3) 0.0597(11) Uani 1 1 d U
H13A H 0.8885 0.8241 0.5379 0.072 Uiso 1 1 d R
C14 C 0.63942(18) 0.6928(2) 0.53461(17) 0.0252(6) Uani 1 1 d U
C15 C 0.8103(3) 1.2417(3) 0.4072(3) 0.0527(10) Uani 1 1 d U
C16 C 0.8427(3) 1.2229(4) 0.4902(3) 0.0546(10) Uani 1 1 d U
H16A H 0.8957 1.1803 0.5193 0.066 Uiso 1 1 d R
C17 C 0.7976(2) 1.2663(3) 0.5322(2) 0.0397(8) Uani 1 1 d U
H17B H 0.8194 1.2553 0.5890 0.048 Uiso 1 1 calc R
H17A H 0.7939 0.7934 0.5947 0.048 Uiso 1 1 d R
C18 C 0.72021(19) 1.3259(3) 0.48914(18) 0.0301(6) Uani 1 1 d U
C19 C 0.6892(2) 1.3426(4) 0.4047(2) 0.0429(8) Uani 1 1 d U
C20 C 0.7343(3) 1.3003(4) 0.3634(2) 0.0487(9) Uani 1 1 d U
H20A H 0.7125 1.3121 0.3049 0.058 Uiso 1 1 d R
C21 C 0.67071(18) 1.3758(3) 0.53228(17) 0.0264(6) Uani 1 1 d U
C22 C 1.25629(19) 0.9495(3) 0.34274(19) 0.0348(7) Uani 1 1 d U
H22A H 1.2078 0.9882 0.3445 0.042 Uiso 1 1 d R
C23 C 1.33574(19) 0.9757(3) 0.40521(19) 0.0346(7) Uani 1 1 d U
H23A H 1.3414 1.0306 0.4490 0.042 Uiso 1 1 d R
C24 C 1.40728(18) 0.9237(3) 0.40526(17) 0.0279(6) Uani 1 1 d U
C25 C 1.3945(2) 0.8432(3) 0.3407(2) 0.0353(7) Uani 1 1 d U
H25A H 1.4422 0.8033 0.3382 0.042 Uiso 1 1 d R
C26 C 1.3132(2) 0.8217(3) 0.2805(2) 0.0365(7) Uani 1 1 d U
H26A H 1.3058 0.7656 0.2367 0.044 Uiso 1 1 d R
C27 C 1.49715(19) 0.9505(3) 0.46896(19) 0.0328(7) Uani 1 1 d U
Co1 Co 1.11987(2) 0.81689(3) 0.19384(2) 0.02226(11) Uani 1 1 d U
Co2 Co 1.0000 1.0000 0.0000 0.01930(12) Uani 1 2 d SU
N1 N 1.24323(15) 0.8735(2) 0.28025(15) 0.0299(5) Uani 1 1 d U
O1 O 1.06194(13) 0.8709(2) 0.26923(13) 0.0325(5) Uani 1 1 d U
O2 O 1.04412(17) 1.0732(2) 0.24536(16) 0.0460(6) Uani 1 1 d U
O3 O 0.8634(2) 0.7692(3) 0.3889(2) 0.0763(9) Uani 1 1 d U
O4 O 0.8567(2) 1.2138(3) 0.3629(2) 0.0750(9) Uani 1 1 d U
O5 O 0.59087(12) 1.3879(2) 0.48782(12) 0.0318(5) Uani 1 1 d U
O6 O 0.70771(13) 1.4049(2) 0.60663(12) 0.0355(5) Uani 1 1 d U
O7 O 0.56863(13) 0.64591(19) 0.48938(12) 0.0298(4) Uani 1 1 d U
O8 O 0.66696(13) 0.71983(19) 0.60947(12) 0.0300(4) Uani 1 1 d U
O9 O 1.00590(14) 0.7264(2) 0.12115(13) 0.0365(5) Uani 1 1 d U
H9A H 0.9606 0.7692 0.1019 0.044 Uiso 1 1 d R
H9B H 0.9998 0.6541 0.1356 0.044 Uiso 1 1 d R
O10 O 1.15289(15) 0.6423(2) 0.25088(14) 0.0413(5) Uani 1 1 d U
H10A H 1.1130 0.5919 0.2434 0.050 Uiso 1 1 d R
H10B H 1.1964 0.6372 0.2973 0.050 Uiso 1 1 d R
O11 O 1.08301(12) 0.99517(16) 0.13191(11) 0.0226(4) Uani 1 1 d U
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 126.3(2) . .
O2 C1 C2 116.6(3) . .
O1 C1 C2 117.1(2) . .
C7 C2 C3 120.5(3) . .
C7 C2 C1 118.8(3) . .
C3 C2 C1 120.6(3) . .
C2 C3 C4 118.7(3) . .
C2 C3 H3A 120.7 . .
C4 C3 H3A 120.6 . .
O3 C4 C5 124.0(3) . .
O3 C4 C3 114.0(3) . .
C5 C4 C3 122.0(3) . .
C4 C5 C6 117.8(3) . .
C4 C5 H5A 120.9 . .
C6 C5 H5A 121.3 . .
O4 C6 C7 114.5(3) . .
O4 C6 C5 123.7(3) . .
C7 C6 C5 121.6(3) . .
C2 C7 C6 119.3(3) . .
C2 C7 H7A 120.2 . .
C6 C7 H7A 120.5 . .
C13 C8 C9 120.9(3) . .
C13 C8 O3 120.5(4) . .
C9 C8 O3 118.3(4) . .
C8 C9 C10 120.0(4) . .
C8 C9 H9C 119.8 . .
C10 C9 H9C 120.2 . .
C9 C10 C11 120.2(4) . .
C9 C10 H10C 119.9 . .
C11 C10 H10C 119.9 . .
C12 C11 C10 118.8(3) . .
C12 C11 C14 121.0(3) . .
C10 C11 C14 120.2(3) . .
C11 C12 C13 120.9(3) . .
C11 C12 H17A 119.4 . .
C13 C12 H17A 119.6 . .
C8 C13 C12 119.1(4) . .
C8 C13 H13A 120.4 . .
C12 C13 H13A 120.4 . .
O7 C14 O8 126.7(2) . .
O7 C14 C11 117.0(2) . .
O8 C14 C11 116.3(2) . .
C20 C15 C16 122.0(3) . .
C20 C15 O4 115.6(3) . .
C16 C15 O4 122.0(4) . .
C15 C16 C17 119.1(3) . .
C15 C16 H16A 120.4 . .
C17 C16 H16A 120.5 . .
C18 C17 C16 119.9(3) . .
C18 C17 H17B 120.0 . .
C16 C17 H17B 120.0 . .
C19 C18 C17 119.2(3) . .
C19 C18 C21 119.2(3) . .
C17 C18 C21 121.5(3) . .
C18 C19 C20 120.7(3) . .
C18 C19 H8A 119.7 . .
C20 C19 H8A 119.6 . .
C15 C20 C19 119.0(3) . .
C15 C20 H20A 120.6 . .
C19 C20 H20A 120.4 . .
O6 C21 O5 123.8(3) . .
O6 C21 C18 120.4(3) . .
O5 C21 C18 115.7(2) . .
N1 C22 C23 123.6(3) . .
N1 C22 H22A 118.4 . .
C23 C22 H22A 118.0 . .
C24 C23 C22 120.3(3) . .
C24 C23 H23A 119.5 . .
C22 C23 H23A 120.2 . .
C23 C24 C25 116.6(3) . .
C23 C24 C27 124.2(3) . .
C25 C24 C27 119.1(3) . .
C26 C25 C24 119.7(3) . .
C26 C25 H25A 120.2 . .
C24 C25 H25A 120.1 . .
N1 C26 C25 123.5(3) . .
N1 C26 H26A 118.1 . .
C25 C26 H26A 118.4 . .
C24 C27 C27 113.9(3) . 3_876
O8 Co1 O9 91.50(9) 4_675 .
O8 Co1 O1 172.79(8) 4_675 .
O9 Co1 O1 86.54(9) . .
O8 Co1 O10 94.18(9) 4_675 .
O9 Co1 O10 82.08(9) . .
O1 Co1 O10 92.42(9) . .
O8 Co1 N1 89.49(9) 4_675 .
O9 Co1 N1 168.19(9) . .
O1 Co1 N1 93.84(9) . .
O10 Co1 N1 86.11(9) . .
O8 Co1 O11 85.33(7) 4_675 .
O9 Co1 O11 96.48(8) . .
O1 Co1 O11 88.00(7) . .
O10 Co1 O11 178.47(8) . .
N1 Co1 O11 95.33(9) . .
O7 Co2 O7 180.00(11) 4_675 2_655
O7 Co2 O5 93.51(8) 4_675 2_645
O7 Co2 O5 86.49(8) 2_655 2_645
O7 Co2 O5 86.49(8) 4_675 4_685
O7 Co2 O5 93.51(8) 2_655 4_685
O5 Co2 O5 180.00(11) 2_645 4_685
O7 Co2 O11 92.99(7) 4_675 3_775
O7 Co2 O11 87.01(7) 2_655 3_775
O5 Co2 O11 87.58(7) 2_645 3_775
O5 Co2 O11 92.42(7) 4_685 3_775
O7 Co2 O11 87.01(7) 4_675 .
O7 Co2 O11 92.99(7) 2_655 .
O5 Co2 O11 92.42(7) 2_645 .
O5 Co2 O11 87.58(7) 4_685 .
O11 Co2 O11 180.0 3_775 .
C22 N1 C26 116.1(3) . .
C22 N1 Co1 122.7(2) . .
C26 N1 Co1 120.6(2) . .
C1 O1 Co1 128.36(18) . .
C4 O3 C8 120.7(3) . .
C6 O4 C15 123.0(3) . .
C21 O5 Co2 131.81(18) . 2_655
C14 O7 Co2 134.93(18) . 2_645
C14 O8 Co1 131.39(18) . 4_576
Co1 O9 H9A 117.3 . .
Co1 O9 H9B 117.3 . .
H9A O9 H9B 114.3 . .
Co1 O10 H10A 118.3 . .
Co1 O10 H10B 118.2 . .
H10A O10 H10B 115.5 . .
Co2 O11 Co1 118.97(8) . .
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(4) .
C1 O1 1.264(4) .
C1 C2 1.518(4) .
C2 C7 1.385(4) .
C2 C3 1.387(4) .
C3 C4 1.389(4) .
C3 H3A 0.9601 .
C4 O3 1.379(4) .
C4 C5 1.381(5) .
C5 C6 1.389(5) .
C5 H5A 0.9601 .
C6 O4 1.368(4) .
C6 C7 1.382(4) .
C7 H7A 0.9600 .
C8 C13 1.370(6) .
C8 C9 1.371(6) .
C8 O3 1.397(4) .
C9 C10 1.379(5) .
C9 H9C 0.9601 .
C10 C11 1.387(4) .
C10 H10C 0.9300 .
C11 C12 1.386(4) .
C11 C14 1.510(4) .
C12 C13 1.382(5) .
C12 H17A 0.9191 .
C13 H13A 0.9601 .
C14 O7 1.252(3) .
C14 O8 1.253(3) .
C15 C20 1.368(5) .
C15 C16 1.364(6) .
C15 O4 1.399(4) .
C16 C17 1.394(4) .
C16 H16A 0.9600 .
C17 C18 1.389(4) .
C17 H17B 0.9300 .
C18 C19 1.386(4) .
C18 C21 1.498(4) .
C19 C20 1.380(4) .
C19 H8A 0.9545 .
C20 H20A 0.9601 .
C21 O6 1.246(3) .
C21 O5 1.274(3) .
C22 N1 1.335(4) .
C22 C23 1.379(4) .
C22 H22A 0.9599 .
C23 C24 1.373(4) .
C23 H23A 0.9601 .
C24 C25 1.394(4) .
C24 C27 1.511(4) .
C25 C26 1.376(4) .
C25 H25A 0.9600 .
C26 N1 1.345(4) .
C26 H26A 0.9600 .
C27 C27 1.525(6) 3_876
Co1 O8 2.0644(19) 4_675
Co1 O9 2.087(2) .
Co1 O1 2.1067(19) .
Co1 O10 2.116(2) .
Co1 N1 2.121(2) .
Co1 O11 2.1892(18) .
Co2 O7 2.0496(19) 4_675
Co2 O7 2.0496(19) 2_655
Co2 O5 2.0905(19) 2_645
Co2 O5 2.0905(19) 4_685
Co2 O11 2.1744(18) 3_775
Co2 O11 2.1745(18) .
O5 Co2 2.0905(19) 2_655
O7 Co2 2.0496(19) 2_645
O8 Co1 2.0644(19) 4_576
O9 H9A 0.8500 .
O9 H9B 0.8500 .
O10 H10A 0.8500 .
O10 H10B 0.8502 .
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 1.000 351 90 ' '
2 0.000 0.500 0.500 352 90 ' '
