#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/74/4507461.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_4507461
loop_
_publ_author_name
'Karra, Jagadeswara R.'
'Huang, You-Gui'
'Walton, Krista S.'
_publ_section_title
;
 Synthesis, Characterization, and Adsorption Studies of Nickel(II),
 Zinc(II), and Magnesium(II) Coordination Frameworks of BTTB
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1075
_journal_paper_doi               10.1021/cg3013393
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C21 H18 Ni0.50 O7'
_chemical_formula_sum            'C21 H18 Ni0.5 O7'
_chemical_formula_weight         411.71
_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                95.441(4)
_cell_angle_beta                 98.941(4)
_cell_angle_gamma                103.448(4)
_cell_formula_units_Z            2
_cell_length_a                   6.2836(16)
_cell_length_b                   10.732(3)
_cell_length_c                   14.356(4)
_cell_measurement_temperature    173(2)
_cell_volume                     921.4(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD '
_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  0.0849
_diffrn_reflns_av_sigmaI/netI    0.1061
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18553
_diffrn_reflns_theta_full        30.65
_diffrn_reflns_theta_max         30.65
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1371P)²+0.2351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2553
_reflns_number_gt                3345
_reflns_number_total             5623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3013393_si_004.cif
_cod_data_source_block           e:\oldc-2~1\reddy\reddy-14\reddy_14\r
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C21 H18 Ni0.50 O7'
_cod_database_code               4507461
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
Ni1 Ni 0.5000 1.0000 0.0000 0.0231(2) Uani 1 2 d S
O1 O 0.3911(5) 0.8665(3) 0.0839(2) 0.0277(6) Uani 1 1 d .
C1 C 0.1556(7) 0.7601(4) 0.1799(3) 0.0256(8) Uani 1 1 d .
O2 O 0.0248(5) 0.8365(3) 0.0382(2) 0.0285(6) Uani 1 1 d .
C2 C 0.3352(7) 0.7435(4) 0.2442(3) 0.0293(9) Uani 1 1 d .
H2 H 0.4832 0.7773 0.2353 0.035 Uiso 1 1 calc R
O3 O 0.6849(5) 0.1232(3) 0.2249(2) 0.0360(7) Uani 1 1 d .
C3 C 0.2969(7) 0.6778(4) 0.3208(3) 0.0303(9) Uani 1 1 d .
H3 H 0.4195 0.6664 0.3640 0.036 Uiso 1 1 calc R
O4 O 0.4408(5) 0.1369(3) 0.09791(19) 0.0299(7) Uani 1 1 d .
C4 C 0.0805(7) 0.6278(4) 0.3355(3) 0.0223(8) Uani 1 1 d .
O5 O 0.1859(5) 0.9806(3) -0.07858(19) 0.0262(6) Uani 1 1 d .
C5 C -0.0961(7) 0.6463(4) 0.2719(3) 0.0293(9) Uani 1 1 d .
H5 H -0.2440 0.6136 0.2814 0.035 Uiso 1 1 calc R
O6 O -0.1648(17) 0.9317(13) 0.4312(8) 0.203(5) Uani 1 1 d .
C6 C -0.0609(7) 0.7115(4) 0.1948(3) 0.0287(9) Uani 1 1 d .
H6 H -0.1839 0.7232 0.1520 0.034 Uiso 1 1 calc R
O7 O 0.4873(9) 0.5101(5) -0.0978(3) 0.0753(14) Uani 1 1 d .
C7 C 0.0387(6) 0.5583(4) 0.4180(3) 0.0212(7) Uani 1 1 d .
C18 C 0.6904(13) 0.5094(8) -0.0381(5) 0.0716(19) Uani 1 1 d .
H18A H 0.7731 0.5993 -0.0117 0.086 Uiso 1 1 calc R
H18B H 0.7840 0.4710 -0.0760 0.086 Uiso 1 1 calc R
C8 C -0.0749(6) 0.6078(3) 0.4827(2) 0.0210(7) Uani 1 1 d .
C19 C 0.3567(14) 0.5677(7) -0.0420(5) 0.0740(19) Uani 1 1 d .
H19A H 0.2149 0.5695 -0.0824 0.089 Uiso 1 1 calc R
H19B H 0.4381 0.6578 -0.0158 0.089 Uiso 1 1 calc R
C9 C 0.1139(6) 0.4472(4) 0.4352(2) 0.0204(7) Uani 1 1 d .
C20 C 0.058(2) 0.9978(11) 0.4145(7) 0.128(4) Uani 1 1 d .
H20A H 0.1184 0.9346 0.3788 0.154 Uiso 1 1 calc R
H20B H 0.0428 1.0666 0.3746 0.154 Uiso 1 1 calc R
C10 C 0.2259(7) 0.3824(4) 0.3688(3) 0.0227(8) Uani 1 1 d .
C21 C -0.2086(17) 0.9478(16) 0.5023(9) 0.147(6) Uani 1 1 d .
H21A H -0.2911 0.8623 0.5146 0.177 Uiso 1 1 calc R
H21B H -0.3174 1.0014 0.4955 0.177 Uiso 1 1 calc R
C11 C 0.1402(7) 0.3537(4) 0.2717(3) 0.0256(8) Uani 1 1 d .
H11 H 0.0138 0.3822 0.2461 0.031 Uiso 1 1 calc R
C12 C 0.2373(7) 0.2840(4) 0.2118(3) 0.0269(8) Uani 1 1 d .
H12 H 0.1775 0.2651 0.1456 0.032 Uiso 1 1 calc R
C13 C 0.4215(7) 0.2418(4) 0.2484(3) 0.0239(8) Uani 1 1 d .
C14 C 0.5116(7) 0.2725(4) 0.3448(3) 0.0288(9) Uani 1 1 d .
H14 H 0.6406 0.2461 0.3700 0.035 Uiso 1 1 calc R
C15 C 0.4140(7) 0.3408(4) 0.4035(3) 0.0258(8) Uani 1 1 d .
H15 H 0.4759 0.3605 0.4695 0.031 Uiso 1 1 calc R
C16 C 0.1929(7) 0.8259(4) 0.0944(3) 0.0259(8) Uani 1 1 d .
C17 C 0.5172(7) 0.1631(4) 0.1841(3) 0.0272(9) 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'
Ni Ni 0.3393 1.1124 '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'
H H 0.0000 0.0000 '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
O1 Ni1 O1 179.999(1) 2_675 .
O1 Ni1 O5 93.85(11) 2_675 2_675
O1 Ni1 O5 86.15(11) . 2_675
O1 Ni1 O5 86.15(11) 2_675 .
O1 Ni1 O5 93.85(11) . .
O5 Ni1 O5 180.0 2_675 .
O1 Ni1 O4 87.34(12) 2_675 2_665
O1 Ni1 O4 92.66(12) . 2_665
O5 Ni1 O4 89.33(11) 2_675 2_665
O5 Ni1 O4 90.67(11) . 2_665
O1 Ni1 O4 92.66(12) 2_675 1_565
O1 Ni1 O4 87.34(12) . 1_565
O5 Ni1 O4 90.67(11) 2_675 1_565
O5 Ni1 O4 89.33(11) . 1_565
O4 Ni1 O4 180.000(1) 2_665 1_565
C16 O1 Ni1 125.9(2) . .
C6 C1 C2 119.4(3) . .
C6 C1 C16 119.8(4) . .
C2 C1 C16 120.8(4) . .
C3 C2 C1 119.9(4) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C2 C3 C4 121.0(4) . .
C2 C3 H3 119.5 . .
C4 C3 H3 119.5 . .
C17 O4 Ni1 128.4(3) . 1_545
C5 C4 C3 118.5(3) . .
C5 C4 C7 120.3(4) . .
C3 C4 C7 121.2(3) . .
C6 C5 C4 121.3(4) . .
C6 C5 H5 119.4 . .
C4 C5 H5 119.4 . .
C21 O6 C20 119.8(10) . .
C5 C6 C1 119.9(4) . .
C5 C6 H6 120.0 . .
C1 C6 H6 120.0 . .
C18 O7 C19 108.6(5) . .
C8 C7 C9 118.8(3) . .
C8 C7 C4 118.1(3) . .
C9 C7 C4 123.0(3) . .
O7 C18 C19 110.2(6) . 2_665
O7 C18 H18A 109.6 . .
C19 C18 H18A 109.6 2_665 .
O7 C18 H18B 109.6 . .
C19 C18 H18B 109.6 2_665 .
H18A C18 H18B 108.1 . .
C7 C8 C9 122.5(3) . 2_566
O7 C19 C18 109.4(6) . 2_665
O7 C19 H19A 109.8 . .
C18 C19 H19A 109.8 2_665 .
O7 C19 H19B 109.8 . .
C18 C19 H19B 109.8 2_665 .
H19A C19 H19B 108.2 . .
C8 C9 C7 118.7(3) 2_566 .
C8 C9 C10 117.9(3) 2_566 .
C7 C9 C10 123.4(3) . .
C21 C20 O6 113.4(8) 2_576 .
C21 C20 H20A 108.9 2_576 .
O6 C20 H20A 108.9 . .
C21 C20 H20B 108.9 2_576 .
O6 C20 H20B 108.9 . .
H20A C20 H20B 107.7 . .
C11 C10 C15 118.0(3) . .
C11 C10 C9 121.6(3) . .
C15 C10 C9 120.3(3) . .
O6 C21 C20 125.2(11) . 2_576
O6 C21 H21A 106.0 . .
C20 C21 H21A 106.0 2_576 .
O6 C21 H21B 106.0 . .
C20 C21 H21B 106.0 2_576 .
H21A C21 H21B 106.3 . .
C12 C11 C10 120.7(4) . .
C12 C11 H11 119.6 . .
C10 C11 H11 119.6 . .
C13 C12 C11 120.1(4) . .
C13 C12 H12 120.0 . .
C11 C12 H12 120.0 . .
C12 C13 C14 119.7(4) . .
C12 C13 C17 119.3(3) . .
C14 C13 C17 121.0(4) . .
C15 C14 C13 119.9(4) . .
C15 C14 H14 120.1 . .
C13 C14 H14 120.1 . .
C14 C15 C10 121.6(4) . .
C14 C15 H15 119.2 . .
C10 C15 H15 119.2 . .
O1 C16 O2 124.8(3) . .
O1 C16 C1 117.2(3) . .
O2 C16 C1 118.0(4) . .
O4 C17 O3 123.0(4) . .
O4 C17 C13 121.6(4) . .
O3 C17 C13 115.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.025(3) 2_675
Ni1 O1 2.025(3) .
Ni1 O5 2.070(3) 2_675
Ni1 O5 2.070(3) .
Ni1 O4 2.073(3) 2_665
Ni1 O4 2.073(3) 1_565
O1 C16 1.258(5) .
C1 C6 1.396(6) .
C1 C2 1.399(6) .
C1 C16 1.495(5) .
O2 C16 1.260(5) .
C2 C3 1.384(5) .
C2 H2 0.9500 .
O3 C17 1.305(5) .
C3 C4 1.397(6) .
C3 H3 0.9500 .
O4 C17 1.236(5) .
O4 Ni1 2.073(3) 1_545
C4 C5 1.389(6) .
C4 C7 1.483(5) .
C5 C6 1.384(5) .
C5 H5 0.9500 .
O6 C21 1.107(13) .
O6 C20 1.483(14) .
C6 H6 0.9500 .
O7 C18 1.424(9) .
O7 C19 1.430(8) .
C7 C8 1.394(5) .
C7 C9 1.410(5) .
C18 C19 1.505(9) 2_665
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C8 C9 1.398(5) 2_566
C19 C18 1.505(9) 2_665
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C9 C8 1.398(5) 2_566
C9 C10 1.483(5) .
C20 C21 1.385(15) 2_576
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C10 C11 1.391(5) .
C10 C15 1.396(5) .
C21 C20 1.385(15) 2_576
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C11 C12 1.388(5) .
C11 H11 0.9500 .
C12 C13 1.386(5) .
C12 H12 0.9500 .
C13 C14 1.388(6) .
C13 C17 1.479(5) .
C14 C15 1.370(5) .
C14 H14 0.9500 .
C15 H15 0.9500 .
