#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:40:19 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233316 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348757.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_4348757
loop_
_publ_author_name
'Ugale, Bharat'
'Dhankhar, Sandeep Singh'
'Nagaraja, C. M.'
_publ_section_title
;
 Construction of 3-Fold-Interpenetrated Three-Dimensional Metal-Organic
 Frameworks of Nickel(II) for Highly Efficient Capture and Conversion of
 Carbon Dioxide.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9757
_journal_page_last               9766
_journal_paper_doi               10.1021/acs.inorgchem.6b01569
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C18 H20 N2 Ni O8'
_chemical_formula_sum            'C18 H20 N2 Ni O8'
_chemical_formula_weight         451.07
_chemical_name_common            Ni-muc-bpaa
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 101.6930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.4247(12)
_cell_length_b                   13.9402(4)
_cell_length_c                   9.4516(3)
_cell_measurement_reflns_used    135117
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.3
_cell_volume                     4570.6(2)
_computing_cell_refinement       'APEX2 (Bruker, 2014); SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014);XPREP(Sheldrick,2014)'
_computing_molecular_graphics    'Ortep, Pluton, mercury, Olex2'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.233
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            132135
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/2
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_meas      1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.015
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1494P)²+13.3842P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4650
_reflns_number_total             5714
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01569_si_002.cif
_cod_data_source_block           Compound1Ni
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4348757
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.842
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ni1 Ni 0.86393(2) 0.29425(3) 0.16184(5) 0.02976(19) Uani 1 1 d . .
O2W O 0.89827(9) 0.3059(2) 0.3696(3) 0.0448(7) Uani 1 1 d . .
H2WA H 0.8981 0.2529 0.4142 0.067 Uiso 1 1 d R U
H2WB H 0.8893 0.3500 0.4157 0.067 Uiso 1 1 d R U
O1AA O 0.83504(8) 0.1770(2) 0.2159(3) 0.0427(6) Uani 1 1 d . .
O3 O 0.82037(8) 0.3782(2) 0.2147(3) 0.0433(6) Uani 1 1 d . .
O4 O 0.85215(10) 0.4430(2) 0.4204(3) 0.0542(8) Uani 1 1 d . .
O1W O 0.88990(9) 0.4217(2) 0.1049(4) 0.0482(7) Uani 1 1 d . .
H1WA H 0.8999 0.4526 0.1810 0.072 Uiso 1 1 d R U
H1WB H 0.8728 0.4564 0.0521 0.072 Uiso 1 1 d R U
O2AA O 0.86800(11) 0.1406(3) 0.4348(4) 0.0681(10) Uani 1 1 d . .
N2 N 0.83261(9) 0.2833(2) -0.0483(3) 0.0326(6) Uani 1 1 d . .
N1 N 0.90700(10) 0.2070(2) 0.1065(4) 0.0433(8) Uani 1 1 d . .
C15 C 0.77403(11) 0.2457(3) -0.2123(4) 0.0364(7) Uani 1 1 d . .
H15 H 0.7486 0.2249 -0.2265 0.044 Uiso 1 1 calc R U
C5 C 0.78796(12) 0.4901(3) 0.3347(5) 0.0425(9) Uani 1 1 d . .
H5 H 0.7893 0.5275 0.4170 0.051 Uiso 1 1 calc R U
C14 C 0.79092(12) 0.2672(4) -0.3300(4) 0.0478(10) Uani 1 1 d . .
C3 C 0.77756(12) 0.0487(3) 0.2478(5) 0.0427(9) Uani 1 1 d . .
H3 H 0.7762 0.0809 0.1607 0.051 Uiso 1 1 calc R U
C18 C 0.79593(10) 0.2558(3) -0.0747(4) 0.0342(7) Uani 1 1 d . .
H18 H 0.7845 0.2427 0.0034 0.041 Uiso 1 1 calc R U
C2 C 0.80973(13) 0.0599(3) 0.3473(5) 0.0506(10) Uani 1 1 d . .
H2 H 0.8134 0.0220 0.4299 0.061 Uiso 1 1 calc R U
C4 C 0.75560(12) 0.4912(3) 0.2381(5) 0.0419(8) Uani 1 1 d . .
H4 H 0.7538 0.4532 0.1562 0.050 Uiso 1 1 calc R U
C1 C 0.84000(12) 0.1306(3) 0.3314(5) 0.0422(8) Uani 1 1 d . .
C17 C 0.84842(12) 0.3031(4) -0.1618(5) 0.0476(10) Uani 1 1 d . .
H17 H 0.8741 0.3225 -0.1446 0.057 Uiso 1 1 calc R U
C6 C 0.82283(11) 0.4329(3) 0.3218(4) 0.0383(8) Uani 1 1 d . .
C16 C 0.82890(14) 0.2963(4) -0.3018(5) 0.0571(13) Uani 1 1 d . .
H16 H 0.8411 0.3111 -0.3773 0.068 Uiso 1 1 calc R U
C11 C 0.94264(13) 0.2373(4) 0.1119(6) 0.0607(13) Uani 1 1 d . .
H11 H 0.9492 0.2989 0.1458 0.073 Uiso 1 1 calc R U
C7 C 0.89883(15) 0.1180(4) 0.0601(7) 0.0668(15) Uani 1 1 d . .
H7 H 0.8742 0.0946 0.0592 0.080 Uiso 1 1 calc R U
C8 C 0.9245(2) 0.0591(5) 0.0137(10) 0.098(3) Uani 1 1 d . .
H8 H 0.9173 -0.0028 -0.0169 0.117 Uiso 1 1 calc R U
C13 C 0.76840(16) 0.2651(8) -0.4851(6) 0.100(3) Uani 1 1 d . .
H13A H 0.7687 0.3296 -0.5232 0.120 Uiso 1 1 calc R U
H13B H 0.7827 0.2250 -0.5397 0.120 Uiso 1 1 calc R U
C10 C 0.97052(18) 0.1815(6) 0.0695(10) 0.093(2) Uani 1 1 d . .
H10 H 0.9956 0.2043 0.0794 0.111 Uiso 1 1 calc R U
C9 C 0.9609(2) 0.0914(6) 0.0122(11) 0.101(3) Uani 1 1 d . .
C12 C 0.9905(3) 0.0311(8) -0.0557(11) 0.116(3) Uani 1 1 d . .
H12A H 0.9771 -0.0058 -0.1377 0.139 Uiso 1 1 calc R U
H12B H 1.0089 0.0730 -0.0879 0.139 Uiso 1 1 calc R U
O3W O 0.9304(2) 0.5419(6) 0.3251(10) 0.166(3) Uani 1 1 d G .
O4W O 0.9159(4) 0.1554(8) 0.6986(12) 0.320(10) Uani 1 1 d G .
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'
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'
N N 0.0061 0.0033 '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
O1AA Ni1 N2 89.03(12) . .
O1AA Ni1 O3 87.48(12) . .
N2 Ni1 O3 89.55(11) . .
O1AA Ni1 O2W 93.01(12) . .
N2 Ni1 O2W 176.93(11) . .
O3 Ni1 O2W 92.83(11) . .
O1AA Ni1 N1 91.45(13) . .
N2 Ni1 N1 89.65(13) . .
O3 Ni1 N1 178.67(13) . .
O2W Ni1 N1 88.01(13) . .
O1AA Ni1 O1W 175.61(12) . .
N2 Ni1 O1W 89.64(12) . .
O3 Ni1 O1W 88.34(12) . .
O2W Ni1 O1W 88.49(12) . .
N1 Ni1 O1W 92.72(13) . .
C1 O1AA Ni1 130.0(3) . .
C6 O3 Ni1 127.0(3) . .
C18 N2 C17 117.5(3) . .
C18 N2 Ni1 120.9(2) . .
C17 N2 Ni1 121.6(3) . .
C11 N1 C7 116.9(4) . .
C11 N1 Ni1 122.9(3) . .
C7 N1 Ni1 120.2(3) . .
C18 C15 C14 118.6(4) . .
C4 C5 C6 124.7(4) . .
C16 C14 C15 117.9(4) . .
C16 C14 C13 119.5(4) . .
C15 C14 C13 122.5(4) . .
C2 C3 C4 126.3(4) . 4_645
N2 C18 C15 123.2(3) . .
C3 C2 C1 122.5(4) . .
C5 C4 C3 123.5(4) . 4_655
O1AA C1 O2AA 124.9(4) . .
O1AA C1 C2 117.1(4) . .
O2AA C1 C2 118.0(4) . .
N2 C17 C16 123.4(4) . .
O4 C6 O3 125.3(4) . .
O4 C6 C5 116.9(3) . .
O3 C6 C5 117.7(4) . .
C17 C16 C14 119.4(4) . .
N1 C11 C10 123.0(6) . .
N1 C7 C8 123.7(5) . .
C7 C8 C9 119.8(6) . .
C13 C13 C14 120.3(7) 7_654 .
C11 C10 C9 119.4(6) . .
C8 C9 C10 117.0(6) . .
C8 C9 C12 122.2(8) . .
C10 C9 C12 120.8(8) . .
C12 C12 C9 106.1(9) 5_755 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1AA 2.047(3) .
Ni1 N2 2.075(3) .
Ni1 O3 2.076(3) .
Ni1 O2W 2.096(3) .
Ni1 N1 2.098(3) .
Ni1 O1W 2.120(3) .
O1AA C1 1.250(5) .
O3 C6 1.257(5) .
O4 C6 1.255(5) .
O2AA C1 1.251(5) .
N2 C18 1.329(5) .
N2 C17 1.336(5) .
N1 C11 1.322(6) .
N1 C7 1.328(6) .
C15 C18 1.380(5) .
C15 C14 1.398(5) .
C5 C4 1.313(6) .
C5 C6 1.495(5) .
C14 C16 1.378(6) .
C14 C13 1.521(6) .
C3 C2 1.332(6) .
C3 C4 1.450(5) 4_645
C2 C1 1.486(6) .
C4 C3 1.450(5) 4_655
C17 C16 1.366(6) .
C11 C10 1.378(8) .
C7 C8 1.361(7) .
C8 C9 1.368(11) .
C13 C13 1.344(12) 7_654
C10 C9 1.383(11) .
C9 C12 1.579(10) .
C12 C12 1.424(17) 5_755
