#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/20/4332020.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332020
loop_
_publ_author_name
'Zang, Shuangquan'
'Su, Yang'
'Li, Yizhi'
'Zhu, Huizhen'
'Meng, Qingjin'
_publ_section_title
;
 One Dense and Two Open Chiral Metal−Organic Frameworks: 
 Crystal Structures and Physical Properties
;
_journal_issue                   7
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2972
_journal_page_last               2978
_journal_paper_doi               10.1021/ic0520418
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_sum            'C72 H84 N8 Ni4 O38'
_chemical_formula_weight         1904.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 105.045(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   24.444(12)
_cell_length_b                   8.242(4)
_cell_length_c                   11.259(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2190.6(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5903
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4182
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0589
_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)+(0.060P)²+1.99P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                3387
_reflns_number_total             4182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0520418sup2.cif
_cod_data_source_block           1
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2190.5(18)
_cod_original_sg_symbol_Hall     'C 2y '
_cod_original_sg_symbol_H-M      'C2 '
_cod_database_code               4332020
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Ni1 Ni 0.31435(3) 0.80579(8) 0.56326(6) 0.03373(18) Uani 1 1 d .
C1 C 0.4517(2) 1.0949(7) 0.4447(5) 0.0327(11) Uani 1 1 d .
C2 C 0.4057(2) 1.0896(6) 0.4997(5) 0.0306(11) Uani 1 1 d .
C3 C 0.3565(2) 1.1728(6) 0.4412(4) 0.0271(10) Uani 1 1 d .
C4 C 0.3543(2) 1.2619(6) 0.3359(5) 0.0355(13) Uani 1 1 d .
H4 H 0.3216 1.3201 0.2993 0.043 Uiso 1 1 calc R
C5 C 0.3999(2) 1.2658(6) 0.2842(5) 0.0354(13) Uani 1 1 d .
H5 H 0.3974 1.3238 0.2121 0.042 Uiso 1 1 calc R
C6 C 0.4491(3) 1.1834(8) 0.3398(6) 0.0458(15) Uani 1 1 d .
H6 H 0.4801 1.1876 0.3067 0.055 Uiso 1 1 calc R
C7 C 0.4112(2) 0.9966(8) 0.6173(5) 0.0394(14) Uani 1 1 d .
C8 C 0.3044(2) 1.1648(7) 0.4904(5) 0.0329(11) Uani 1 1 d .
C9 C 0.3571(2) 0.7469(6) 0.3425(5) 0.0283(11) Uani 1 1 d .
H9 H 0.3883 0.7086 0.4020 0.034 Uiso 1 1 calc R
C10 C 0.3599(2) 0.7478(7) 0.2244(5) 0.0353(13) Uani 1 1 d .
H10 H 0.3916 0.7058 0.2044 0.042 Uiso 1 1 calc R
C11 C 0.3152(2) 0.8116(9) 0.1312(4) 0.0341(10) Uani 1 1 d .
C12 C 0.2676(2) 0.8596(6) 0.1681(5) 0.0305(12) Uani 1 1 d .
H12 H 0.2357 0.8975 0.1105 0.037 Uiso 1 1 calc R
C13 C 0.2679(2) 0.8509(7) 0.2888(5) 0.0372(14) Uani 1 1 d .
H13 H 0.2355 0.8840 0.3106 0.045 Uiso 1 1 calc R
C14 C 0.2885(2) 0.9255(7) 0.7970(4) 0.0285(11) Uani 1 1 d .
H14 H 0.2680 1.0042 0.7447 0.034 Uiso 1 1 calc R
C15 C 0.2868(3) 0.9261(7) 0.9193(5) 0.0374(13) Uani 1 1 d .
H15 H 0.2652 1.0042 0.9458 0.045 Uiso 1 1 calc R
C16 C 0.31580(18) 0.8164(8) 1.0010(4) 0.0313(10) Uani 1 1 d .
C17 C 0.3483(2) 0.7012(6) 0.9556(5) 0.0310(11) Uani 1 1 d .
H17 H 0.3691 0.6222 1.0070 0.037 Uiso 1 1 calc R
C18 C 0.3485(2) 0.7092(7) 0.8317(5) 0.0341(12) Uani 1 1 d .
H18 H 0.3709 0.6355 0.8030 0.041 Uiso 1 1 calc R
N1 N 0.31188(18) 0.7979(8) 0.3793(4) 0.0396(10) Uani 1 1 d .
N2 N 0.31799(16) 0.8173(7) 0.7511(4) 0.0320(9) Uani 1 1 d .
O1 O 0.40139(15) 0.8461(4) 0.6139(3) 0.0304(8) Uani 1 1 d .
O2 O 0.43055(16) 1.0746(5) 0.7156(3) 0.0348(8) Uani 1 1 d .
O3 O 0.29588(16) 1.0494(5) 0.5520(3) 0.0302(8) Uani 1 1 d .
O4 O 0.27153(14) 1.2849(5) 0.4624(3) 0.0328(8) Uani 1 1 d .
O5 O 0.5000 1.0036(7) 0.5000 0.0335(11) Uani 1 2 d S
O6 O 0.32919(17) 0.5627(5) 0.5735(3) 0.0347(9) Uani 1 1 d .
H6B H 0.3260 0.5252 0.5017 0.042 Uiso 1 1 d R
H6A H 0.3612 0.5455 0.6167 0.042 Uiso 1 1 d R
O7 O 0.42353(16) 0.4115(5) 0.7068(3) 0.0379(9) Uani 1 1 d .
H7C H 0.4522 0.4447 0.6844 0.045 Uiso 1 1 d R
H7A H 0.4199 0.3097 0.6958 0.045 Uiso 1 1 d R
O8 O 0.50308(16) 0.8376(5) 0.8832(3) 0.0411(10) Uani 1 1 d .
H8A H 0.5350 0.8140 0.9315 0.049 Uiso 1 1 d R
H8B H 0.5078 0.9048 0.8294 0.049 Uiso 1 1 d R
O9 O 0.4218(4) 0.1682(10) 0.9701(8) 0.0423(18) Uani 0.50 1 d P
H9A H 0.4268 0.1559 1.0462 0.051 Uiso 0.50 1 d PR
H9B H 0.3853 0.1567 0.9354 0.051 Uiso 0.50 1 d PR
O10 O 0.49037(17) 0.6198(5) 0.6125(3) 0.0399(9) Uani 1 1 d .
H10A H 0.5218 0.5743 0.6142 0.048 Uiso 1 1 d R
H10C H 0.4965 0.7081 0.6529 0.048 Uiso 1 1 d R
O11 O 0.4623(3) 0.4426(10) 0.0523(7) 0.0377(18) Uani 0.50 1 d P
H11D H 0.4499 0.3498 0.0250 0.045 Uiso 0.50 1 d PR
H11B H 0.4913 0.4661 0.0273 0.045 Uiso 0.50 1 d PR
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'
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
O6 Ni1 O4 94.95(16) . 4_546
O6 Ni1 O3 177.64(19) . .
O4 Ni1 O3 82.70(15) 4_546 .
O6 Ni1 N1 89.1(2) . .
O4 Ni1 N1 95.39(15) 4_546 .
O3 Ni1 N1 91.2(2) . .
O6 Ni1 O1 89.26(15) . .
O4 Ni1 O1 171.20(14) 4_546 .
O3 Ni1 O1 93.06(14) . .
N1 Ni1 O1 92.39(16) . .
O6 Ni1 N2 91.56(19) . .
O4 Ni1 N2 85.40(14) 4_546 .
O3 Ni1 N2 88.22(18) . .
N1 Ni1 N2 178.9(3) . .
O1 Ni1 N2 86.77(14) . .
C6 C1 O5 120.8(4) . .
C6 C1 C2 121.8(5) . .
O5 C1 C2 117.5(4) . .
C3 C2 C1 117.6(5) . .
C3 C2 C7 122.3(4) . .
C1 C2 C7 120.1(5) . .
C4 C3 C2 120.3(4) . .
C4 C3 C8 119.1(5) . .
C2 C3 C8 120.6(4) . .
C3 C4 C5 121.0(5) . .
C3 C4 H4 119.5 . .
C5 C4 H4 119.5 . .
C6 C5 C4 119.9(5) . .
C6 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
C1 C6 C5 119.4(5) . .
C1 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
O2 C7 O1 123.6(5) . .
O2 C7 C2 116.0(5) . .
O1 C7 C2 120.1(5) . .
O3 C8 O4 123.9(5) . .
O3 C8 C3 121.5(5) . .
O4 C8 C3 114.5(5) . .
N1 C9 C10 123.9(5) . .
N1 C9 H9 118.1 . .
C10 C9 H9 118.1 . .
C9 C10 C11 120.7(5) . .
C9 C10 H10 119.7 . .
C11 C10 H10 119.7 . .
C12 C11 C10 115.5(4) . .
C12 C11 C16 121.1(4) . 1_554
C10 C11 C16 123.2(4) . 1_554
C13 C12 C11 119.7(5) . .
C13 C12 H12 120.2 . .
C11 C12 H12 120.2 . .
N1 C13 C12 124.8(5) . .
N1 C13 H13 117.6 . .
C12 C13 H13 117.6 . .
N2 C14 C15 123.0(5) . .
N2 C14 H14 118.5 . .
C15 C14 H14 118.5 . .
C16 C15 C14 121.9(5) . .
C16 C15 H15 119.1 . .
C14 C15 H15 119.1 . .
C15 C16 C17 116.5(4) . .
C15 C16 C11 123.9(5) . 1_556
C17 C16 C11 119.6(5) . 1_556
C18 C17 C16 118.4(5) . .
C18 C17 H17 120.8 . .
C16 C17 H17 120.8 . .
N2 C18 C17 123.9(5) . .
N2 C18 H18 118.1 . .
C17 C18 H18 118.1 . .
C9 N1 C13 115.3(4) . .
C9 N1 Ni1 120.5(4) . .
C13 N1 Ni1 124.1(4) . .
C14 N2 C18 116.2(4) . .
C14 N2 Ni1 122.4(3) . .
C18 N2 Ni1 121.3(4) . .
C7 O1 Ni1 109.7(3) . .
C8 O3 Ni1 136.5(3) . .
C8 O4 Ni1 131.5(4) . 4_556
C1 O5 C1 115.1(6) . 2_656
Ni1 O6 H6B 109.5 . .
Ni1 O6 H6A 109.5 . .
H6B O6 H6A 109.8 . .
H7C O7 H7A 109.8 . .
H8A O8 H8B 109.5 . .
H9A O9 H9B 107.4 . .
H10A O10 H10C 109.5 . .
H11D O11 H11B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O6 2.034(4) .
Ni1 O4 2.051(3) 4_546
Ni1 O3 2.055(4) .
Ni1 N1 2.058(4) .
Ni1 O1 2.081(4) .
Ni1 N2 2.096(4) .
C1 C6 1.375(7) .
C1 O5 1.403(6) .
C1 C2 1.416(7) .
C2 C3 1.393(7) .
C2 C7 1.506(8) .
C3 C4 1.383(7) .
C3 C8 1.517(7) .
C4 C5 1.387(7) .
C4 H4 0.9300 .
C5 C6 1.381(8) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 O2 1.261(7) .
C7 O1 1.261(7) .
C8 O3 1.226(7) .
C8 O4 1.263(7) .
C9 N1 1.345(6) .
C9 C10 1.349(7) .
C9 H9 0.9300 .
C10 C11 1.405(7) .
C10 H10 0.9300 .
C11 C12 1.392(7) .
C11 C16 1.470(6) 1_554
C12 C13 1.359(7) .
C12 H12 0.9300 .
C13 N1 1.347(7) .
C13 H13 0.9300 .
C14 N2 1.333(7) .
C14 C15 1.387(7) .
C14 H14 0.9300 .
C15 C16 1.351(8) .
C15 H15 0.9300 .
C16 C17 1.417(8) .
C16 C11 1.470(6) 1_556
C17 C18 1.397(7) .
C17 H17 0.9300 .
C18 N2 1.350(7) .
C18 H18 0.9300 .
O4 Ni1 2.051(3) 4_556
O5 C1 1.403(6) 2_656
O6 H6B 0.8501 .
O6 H6A 0.8200 .
O7 H7C 0.8499 .
O7 H7A 0.8500 .
O8 H8A 0.8501 .
O8 H8B 0.8501 .
O9 H9A 0.8399 .
O9 H9B 0.8815 .
O10 H10A 0.8500 .
O10 H10C 0.8500 .
O11 H11D 0.8500 .
O11 H11B 0.8500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6B O4 0.85 2.36 2.807(6) 113.0 1_545
O7 H7A O2 0.85 1.96 2.782(6) 162.5 1_545
O6 H6A O7 0.82 1.94 2.707(5) 155.2 .
O7 H7C O10 0.85 2.00 2.765(6) 149.3 .
O8 H8B O2 0.85 2.43 2.964(5) 121.4 .
O11 H11D O9 0.85 1.70 2.544(12) 177.0 1_554
O11 H11B O11 0.85 1.63 2.432(14) 156.2 2_655
