#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/16/4001628.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_4001628
loop_
_publ_author_name
'Yao, Ru-Xin'
'Xu, Xia'
'Zhang, Xian-Ming'
_publ_section_title
;
 Magnetic Modulation and Cation-Exchange in a Series of Isostructural
 (4,8)-Connected Metal--Organic Frameworks with Butterfly-like
 [M4(OH)2(RCO2)8] Building Units
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              303
_journal_paper_doi               10.1021/cm202876r
_journal_volume                  24
_journal_year                    2012
_chemical_formula_sum            'C18 H19 Co0.25 N Ni1.75 O11'
_chemical_formula_weight         542.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.6300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5186(6)
_cell_length_b                   10.7685(5)
_cell_length_c                   14.6323(7)
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.40
_cell_volume                     1993.51(16)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SAINT (Bruker, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex CCD Diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9974
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.924
_exptl_absorpt_correction_T_max  0.8309
_exptl_absorpt_correction_T_min  0.5869
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1091
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.100
_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     289
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0361
_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)+(0.0530P)²+1.0438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3622
_reflns_number_total             4348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm202876r_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4001628
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Co1 Co 0.41053(3) 0.90409(3) 0.46176(2) 0.01479(11) Uani 0.13 1 d P
Ni1 Ni 0.41053(3) 0.90409(3) 0.46176(2) 0.01479(11) Uani 0.87 1 d P
Co2 Co 0.50388(3) 1.01066(3) 0.29220(2) 0.01429(11) Uani 0.13 1 d P
Ni2 Ni 0.50388(3) 1.01066(3) 0.29220(2) 0.01429(11) Uani 0.87 1 d P
N1 N 0.2526(3) 0.0385(3) 0.0550(2) 0.0467(8) Uani 1 1 d .
H1D H 0.2909 -0.0079 0.1064 0.056 Uiso 1 1 calc R
H1E H 0.2722 0.1182 0.0689 0.056 Uiso 1 1 calc R
O1 O 0.30472(15) 1.03122(18) 0.37356(14) 0.0220(4) Uani 1 1 d .
O2 O 0.39011(15) 1.13533(18) 0.29092(15) 0.0201(4) Uani 1 1 d .
O3 O 0.38627(17) 1.40425(19) 0.23872(15) 0.0255(5) Uani 1 1 d .
O4 O 0.31281(18) 1.2844(2) 0.10790(16) 0.0315(5) Uani 1 1 d .
O5 O -0.37998(16) 1.14612(19) 0.34043(14) 0.0238(5) Uani 1 1 d .
O6 O -0.28606(16) 1.15218(19) 0.50123(14) 0.0226(4) Uani 1 1 d .
O7 O -0.36617(15) 1.27744(18) 0.15312(13) 0.0192(4) Uani 1 1 d .
O8 O -0.37188(15) 1.39582(17) 0.27776(14) 0.0195(4) Uani 1 1 d .
O9 O 0.53793(14) 0.95995(17) 0.43124(13) 0.0154(4) Uani 1 1 d .
C1 C 0.1406(4) 0.0263(4) 0.0419(4) 0.0683(14) Uani 1 1 d .
H1A H 0.1297 0.0527 0.1003 0.103 Uiso 1 1 calc R
H1B H 0.1194 -0.0588 0.0287 0.103 Uiso 1 1 calc R
H1C H 0.0992 0.0772 -0.0119 0.103 Uiso 1 1 calc R
C2 C 0.2778(4) -0.0003(5) -0.0324(3) 0.0710(15) Uani 1 1 d .
H2A H 0.3523 0.0089 -0.0189 0.107 Uiso 1 1 calc R
H2B H 0.2393 0.0508 -0.0871 0.107 Uiso 1 1 calc R
H2C H 0.2581 -0.0856 -0.0473 0.107 Uiso 1 1 calc R
C3 C 0.3136(2) 1.1172(2) 0.31966(19) 0.0162(6) Uani 1 1 d .
C4 C 0.2243(2) 1.2092(3) 0.2852(2) 0.0176(6) Uani 1 1 d .
C5 C 0.1399(2) 1.1956(3) 0.3177(2) 0.0211(6) Uani 1 1 d .
H5A H 0.1403 1.1297 0.3589 0.025 Uiso 1 1 calc R
C6 C 0.0550(2) 1.2772(3) 0.2906(2) 0.0208(6) Uani 1 1 d .
C7 C 0.0573(2) 1.3757(3) 0.2290(2) 0.0259(7) Uani 1 1 d .
H7A H 0.0018 1.4323 0.2097 0.031 Uiso 1 1 calc R
C8 C 0.1408(2) 1.3899(3) 0.1964(2) 0.0263(7) Uani 1 1 d .
H8A H 0.1403 1.4559 0.1553 0.032 Uiso 1 1 calc R
C9 C 0.2258(2) 1.3080(3) 0.2237(2) 0.0197(6) Uani 1 1 d .
C10 C 0.3160(2) 1.3317(3) 0.1870(2) 0.0197(6) Uani 1 1 d .
C11 C -0.0339(2) 1.2583(3) 0.3260(2) 0.0185(6) Uani 1 1 d .
C12 C -0.0179(2) 1.2025(3) 0.4166(2) 0.0210(6) Uani 1 1 d .
H12A H 0.0503 1.1816 0.4568 0.025 Uiso 1 1 calc R
C13 C -0.1016(2) 1.1780(3) 0.4474(2) 0.0194(6) Uani 1 1 d .
H13A H -0.0891 1.1405 0.5077 0.023 Uiso 1 1 calc R
C14 C -0.2042(2) 1.2090(2) 0.38887(19) 0.0158(5) Uani 1 1 d .
C15 C -0.2212(2) 1.2702(2) 0.30059(19) 0.0152(5) Uani 1 1 d .
C17 C -0.1371(2) 1.2930(3) 0.2694(2) 0.0188(6) Uani 1 1 d .
H17A H -0.1496 1.3322 0.2097 0.023 Uiso 1 1 calc R
C18 C -0.2976(2) 1.1655(2) 0.41295(19) 0.0159(6) Uani 1 1 d .
C19 C -0.3293(2) 1.3166(2) 0.2391(2) 0.0163(6) Uani 1 1 d .
O2W O 0.48317(18) 1.0919(2) 0.15084(15) 0.0345(6) Uani 1 1 d .
O1W O 0.49726(18) 0.7398(2) 0.54057(16) 0.0344(6) Uani 1 1 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'
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'
Ni Ni 0.3393 1.1124 '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
O9 Co1 O6 177.52(7) . 3_576
O9 Co1 O1 96.95(8) . .
O6 Co1 O1 84.74(8) 3_576 .
O9 Co1 O9 82.58(8) . 3_676
O6 Co1 O9 95.66(8) 3_576 3_676
O1 Co1 O9 88.76(8) . 3_676
O9 Co1 O7 92.41(8) . 2_545
O6 Co1 O7 89.41(8) 3_576 2_545
O1 Co1 O7 89.46(8) . 2_545
O9 Co1 O7 174.44(7) 3_676 2_545
O9 Co1 O1W 90.96(8) . .
O6 Co1 O1W 87.66(8) 3_576 .
O1 Co1 O1W 167.96(9) . .
O9 Co1 O1W 101.29(8) 3_676 .
O7 Co1 O1W 81.13(8) 2_545 .
O9 Co2 O2 95.27(8) . .
O9 Co2 O3 98.46(8) . 2_645
O2 Co2 O3 166.07(8) . 2_645
O9 Co2 O5 88.31(8) . 1_655
O2 Co2 O5 91.04(8) . 1_655
O3 Co2 O5 87.01(9) 2_645 1_655
O9 Co2 O8 100.69(7) . 2_545
O2 Co2 O8 82.84(8) . 2_545
O3 Co2 O8 96.87(8) 2_645 2_545
O5 Co2 O8 169.51(8) 1_655 2_545
O9 Co2 O2W 170.63(8) . .
O2 Co2 O2W 83.23(9) . .
O3 Co2 O2W 82.83(9) 2_645 .
O5 Co2 O2W 82.47(8) 1_655 .
O8 Co2 O2W 88.33(8) 2_545 .
C1 N1 C2 113.6(4) . .
C1 N1 H1D 108.8 . .
C2 N1 H1D 108.8 . .
C1 N1 H1E 108.8 . .
C2 N1 H1E 108.8 . .
H1D N1 H1E 107.7 . .
C3 O1 Co1 133.25(18) . .
C3 O2 Co2 126.89(17) . .
C10 O3 Ni2 131.89(19) . 2_655
C10 O3 Co2 131.89(19) . 2_655
Ni2 O3 Co2 0.00(2) 2_655 2_655
C18 O5 Ni2 138.01(18) . 1_455
C18 O5 Co2 138.01(18) . 1_455
Ni2 O5 Co2 0.000(15) 1_455 1_455
C18 O6 Ni1 119.61(17) . 3_576
C18 O6 Co1 119.61(17) . 3_576
Ni1 O6 Co1 0.00(2) 3_576 3_576
C19 O7 Ni1 119.36(17) . 2
C19 O7 Co1 119.36(17) . 2
Ni1 O7 Co1 0.000(14) 2 2
C19 O8 Ni2 127.98(17) . 2
C19 O8 Co2 127.98(17) . 2
Ni2 O8 Co2 0.000(14) 2 2
Co2 O9 Co1 113.50(9) . .
Co2 O9 Ni1 118.10(9) . 3_676
Co1 O9 Ni1 97.42(8) . 3_676
Co2 O9 Co1 118.10(9) . 3_676
Co1 O9 Co1 97.42(8) . 3_676
Ni1 O9 Co1 0.000(15) 3_676 3_676
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O1 C3 O2 126.7(3) . .
O1 C3 C4 117.2(2) . .
O2 C3 C4 116.2(2) . .
C5 C4 C9 120.0(3) . .
C5 C4 C3 118.2(2) . .
C9 C4 C3 121.7(2) . .
C6 C5 C4 122.1(3) . .
C6 C5 H5A 119.0 . .
C4 C5 H5A 119.0 . .
C5 C6 C7 117.4(3) . .
C5 C6 C11 120.3(3) . .
C7 C6 C11 122.3(3) . .
C8 C7 C6 120.9(3) . .
C8 C7 H7A 119.6 . .
C6 C7 H7A 119.6 . .
C7 C8 C9 121.6(3) . .
C7 C8 H8A 119.2 . .
C9 C8 H8A 119.2 . .
C8 C9 C4 118.0(3) . .
C8 C9 C10 118.5(2) . .
C4 C9 C10 123.4(2) . .
O4 C10 O3 125.6(3) . .
O4 C10 C9 119.3(3) . .
O3 C10 C9 115.0(3) . .
C17 C11 C12 117.6(3) . .
C17 C11 C6 121.3(3) . .
C12 C11 C6 121.1(3) . .
C13 C12 C11 121.3(3) . .
C13 C12 H12A 119.4 . .
C11 C12 H12A 119.4 . .
C12 C13 C14 120.4(3) . .
C12 C13 H13A 119.8 . .
C14 C13 H13A 119.8 . .
C13 C14 C15 119.1(2) . .
C13 C14 C18 121.3(2) . .
C15 C14 C18 119.2(2) . .
C17 C15 C14 120.1(2) . .
C17 C15 C19 118.7(2) . .
C14 C15 C19 121.2(2) . .
C15 C17 C11 121.3(3) . .
C15 C17 H17A 119.3 . .
C11 C17 H17A 119.3 . .
O6 C18 O5 127.1(3) . .
O6 C18 C14 117.9(2) . .
O5 C18 C14 115.0(2) . .
O7 C19 O8 126.3(2) . .
O7 C19 C15 116.6(2) . .
O8 C19 C15 117.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O9 2.0174(18) .
Co1 O6 2.033(2) 3_576
Co1 O1 2.0699(19) .
Co1 O9 2.0764(18) 3_676
Co1 O7 2.0822(19) 2_545
Co1 O1W 2.209(2) .
Co2 O9 1.9973(18) .
Co2 O2 2.0367(19) .
Co2 O3 2.048(2) 2_645
Co2 O5 2.076(2) 1_655
Co2 O8 2.1153(19) 2_545
Co2 O2W 2.171(2) .
N1 C1 1.464(5) .
N1 C2 1.494(6) .
N1 H1D 0.9000 .
N1 H1E 0.9000 .
O1 C3 1.249(3) .
O2 C3 1.262(3) .
O3 C10 1.257(3) .
O3 Ni2 2.048(2) 2_655
O3 Co2 2.048(2) 2_655
O4 C10 1.251(4) .
O5 C18 1.256(3) .
O5 Ni2 2.0760(19) 1_455
O5 Co2 2.0760(19) 1_455
O6 C18 1.254(3) .
O6 Ni1 2.033(2) 3_576
O6 Co1 2.033(2) 3_576
O7 C19 1.251(3) .
O7 Ni1 2.0822(19) 2
O7 Co1 2.0822(19) 2
O8 C19 1.268(3) .
O8 Ni2 2.1153(19) 2
O8 Co2 2.1153(19) 2
O9 Ni1 2.0764(18) 3_676
O9 Co1 2.0764(18) 3_676
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C4 1.504(4) .
C4 C5 1.391(4) .
C4 C9 1.397(4) .
C5 C6 1.388(4) .
C5 H5A 0.9300 .
C6 C7 1.399(4) .
C6 C11 1.480(4) .
C7 C8 1.380(4) .
C7 H7A 0.9300 .
C8 C9 1.390(4) .
C8 H8A 0.9300 .
C9 C10 1.517(4) .
C11 C17 1.400(4) .
C11 C12 1.401(4) .
C12 C13 1.383(4) .
C12 H12A 0.9300 .
C13 C14 1.390(4) .
C13 H13A 0.9300 .
C14 C15 1.395(4) .
C14 C18 1.501(4) .
C15 C17 1.387(4) .
C15 C19 1.507(4) .
C17 H17A 0.9300 .
