#------------------------------------------------------------------------------
#$Date: 2019-10-29 23:39:13 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/30/4003046.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_4003046
loop_
_publ_author_name
'Ayoub, Ghada'
'Karadeniz, Bahar'
'Howarth, Ashlee J.'
'Farha, Omar K.'
'Đilović, Ivica'
'Germann, Luzia S.'
'Dinnebier, Robert E.'
'Užarević, Krunoslav'
'Friščić, Tomislav'
_publ_section_title
;
 Rational Synthesis of Mixed-Metal Microporous Metal--Organic Frameworks
 with Controlled Composition Using Mechanochemistry
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5494
_journal_paper_doi               10.1021/acs.chemmater.9b01068
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C8 H12 Ni O10, 2(H2 O)'
_chemical_formula_sum            'C8 H16 Ni O12'
_chemical_formula_weight         362.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                89.144(5)
_cell_angle_beta                 87.701(6)
_cell_angle_gamma                67.707(6)
_cell_formula_units_Z            2
_cell_length_a                   6.9497(5)
_cell_length_b                   8.6455(5)
_cell_length_c                   12.4065(9)
_cell_measurement_reflns_used    764
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.1770
_cell_measurement_theta_min      7.7330
_cell_volume                     689.16(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5148
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.994
_diffrn_reflns_theta_max         66.994
_diffrn_reflns_theta_min         3.565
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2454
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0852P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2139
_reflns_number_total             2454
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b01068_si_002.cif
_cod_data_source_block           nidhta
_cod_database_code               4003046
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C11 C 0.4880(4) 0.9171(3) 0.4058(2) 0.0271(5) Uani 1 1 d . .
C12 C 0.3960(4) 1.0923(3) 0.4130(2) 0.0277(5) Uani 1 1 d . .
C13 C 0.5921(4) 0.8270(3) 0.4939(2) 0.0288(5) Uani 1 1 d . .
H13 H 0.6543 0.7110 0.4900 0.035 Uiso 1 1 calc R U
C14 C 0.4717(4) 0.8267(4) 0.3077(2) 0.0295(6) Uani 1 1 d . .
C21 C 0.9022(4) 0.0837(3) 0.4076(2) 0.0269(5) Uani 1 1 d . .
C22 C 0.9092(4) 0.1744(3) 0.4986(2) 0.0274(5) Uani 1 1 d . .
C23 C 1.0055(4) 0.0911(3) 0.5892(2) 0.0274(5) Uani 1 1 d . .
H23 H 1.0093 0.1523 0.6496 0.033 Uiso 1 1 calc R U
C24 C 0.7967(4) 0.1681(3) 0.3079(2) 0.0292(6) Uani 1 1 d . .
Ni1 Ni 0.52856(7) 0.49786(5) 0.20767(3) 0.0271(2) Uani 1 1 d . .
O1W O 0.2618(3) 0.5061(2) 0.29052(13) 0.0342(4) Uani 1 1 d D .
O2W O 0.5219(3) 0.3066(2) 0.10767(14) 0.0320(4) Uani 1 1 d D .
O3W O 0.7845(3) 0.4996(2) 0.11772(17) 0.0414(5) Uani 1 1 d D .
O4W O 0.3402(3) 0.6815(2) 0.10606(13) 0.0321(4) Uani 1 1 d D .
O5W O 0.9023(3) 0.7739(2) 0.12574(12) 0.0463(6) Uani 1 1 d DG .
O6W O 0.8323(5) 0.7803(3) -0.08919(13) 0.0572(7) Uani 1 1 d DG .
O11 O 0.5464(3) 0.6703(2) 0.31000(16) 0.0350(5) Uani 1 1 d . .
O12 O 0.3833(4) 0.9123(3) 0.22689(16) 0.0397(5) Uani 1 1 d . .
O13 O 0.2898(4) 1.1857(3) 0.32899(17) 0.0379(5) Uani 1 1 d . .
H13O H 0.2920 1.1238 0.2791 0.057 Uiso 1 1 calc R U
O21 O 0.7102(3) 0.3265(2) 0.31246(16) 0.0358(5) Uani 1 1 d . .
O22 O 0.7951(4) 0.0850(3) 0.22684(17) 0.0433(5) Uani 1 1 d . .
O23 O 0.8225(4) 0.3449(2) 0.50292(17) 0.0397(5) Uani 1 1 d . .
H23O H 0.7630 0.3813 0.4468 0.060 Uiso 1 1 calc R U
H2WB H 0.4127(3) 0.2868(5) 0.1066(6) 0.048(11) Uiso 1 1 d D .
H4WB H 0.3764(13) 0.6790(6) 0.04049(17) 0.072(15) Uiso 1 1 d D .
H4WA H 0.3509(9) 0.7681(3) 0.1302(3) 0.079(16) Uiso 1 1 d D .
H5WA H 1.0311(3) 0.7483(8) 0.1164(7) 0.083(17) Uiso 1 1 d D .
H5WB H 0.8608(8) 0.8635(4) 0.1610(4) 0.063(14) Uiso 1 1 d D .
H2WA H 0.6030(5) 0.2292(5) 0.1450(4) 0.066(14) Uiso 1 1 d D .
H1WA H 0.2511(14) 0.5503(4) 0.35144(19) 0.046(11) Uiso 1 1 d D .
H3WA H 0.8132(8) 0.5740(3) 0.1480(5) 0.059(13) Uiso 1 1 d D .
H1WB H 0.2610(9) 0.4107(3) 0.3036(4) 0.060(13) Uiso 1 1 d D .
H3WB H 0.8949(6) 0.4141(3) 0.1187(8) 0.074(15) Uiso 1 1 d D .
H6WA H 0.8621(13) 0.7785(6) -0.0241(2) 0.076(15) Uiso 1 1 d D .
H6WB H 0.803(2) 0.8800(3) -0.1085(3) 0.16(3) Uiso 1 1 d D .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C13 C11 C12 118.8(3) . .
C13 C11 C14 119.6(2) . .
C12 C11 C14 121.5(2) . .
O13 C12 C13 118.7(2) . 2_676
O13 C12 C11 120.8(3) . .
C13 C12 C11 120.5(3) 2_676 .
C12 C13 C11 120.7(3) 2_676 .
C12 C13 H13 119.6 2_676 .
C11 C13 H13 119.6 . .
O11 C14 O12 124.0(3) . .
O11 C14 C11 117.7(2) . .
O12 C14 C11 118.3(3) . .
C22 C21 C23 118.8(2) . 2_756
C22 C21 C24 121.8(2) . .
C23 C21 C24 119.4(3) 2_756 .
O23 C22 C23 117.4(2) . .
O23 C22 C21 122.8(2) . .
C23 C22 C21 119.8(2) . .
C22 C23 C21 121.5(3) . 2_756
C22 C23 H23 119.3 . .
C21 C23 H23 119.3 2_756 .
O22 C24 O21 123.4(2) . .
O22 C24 C21 120.8(2) . .
O21 C24 C21 115.8(2) . .
O11 Ni1 O21 85.61(8) . .
O11 Ni1 O1W 89.02(8) . .
O21 Ni1 O1W 91.36(8) . .
O11 Ni1 O3W 91.46(8) . .
O21 Ni1 O3W 92.17(8) . .
O1W Ni1 O3W 176.46(7) . .
O11 Ni1 O4W 91.80(8) . .
O21 Ni1 O4W 177.32(7) . .
O1W Ni1 O4W 87.92(7) . .
O3W Ni1 O4W 88.55(7) . .
O11 Ni1 O2W 176.38(7) . .
O21 Ni1 O2W 90.77(7) . .
O1W Ni1 O2W 91.09(7) . .
O3W Ni1 O2W 88.65(7) . .
O4W Ni1 O2W 91.82(7) . .
Ni1 O1W H1WA 110.9(7) . .
Ni1 O1W H1WB 112.9(4) . .
H1WA O1W H1WB 104.683(18) . .
Ni1 O2W H2WB 119.1(5) . .
Ni1 O2W H2WA 94.5(4) . .
H2WB O2W H2WA 104.683(18) . .
Ni1 O3W H3WA 102.9(5) . .
Ni1 O3W H3WB 118.4(6) . .
H3WA O3W H3WB 104.683(19) . .
Ni1 O4W H4WB 118.6(5) . .
Ni1 O4W H4WA 101.9(3) . .
H4WB O4W H4WA 104.683(18) . .
H5WA O5W H5WB 104.683(19) . .
H6WA O6W H6WB 104.683(18) . .
C14 O11 Ni1 131.89(18) . .
C12 O13 H13O 109.5 . .
C24 O21 Ni1 131.86(18) . .
C22 O23 H23O 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C11 C13 1.391(4) .
C11 C12 1.405(4) .
C11 C14 1.487(4) .
C12 O13 1.366(3) .
C12 C13 1.380(4) 2_676
C13 C12 1.380(4) 2_676
C13 H13 0.9300 .
C14 O11 1.251(3) .
C14 O12 1.269(4) .
C21 C22 1.397(4) .
C21 C23 1.400(4) 2_756
C21 C24 1.496(3) .
C22 O23 1.365(3) .
C22 C23 1.379(4) .
C23 C21 1.400(4) 2_756
C23 H23 0.9300 .
C24 O22 1.247(4) .
C24 O21 1.271(3) .
Ni1 O11 2.015(2) .
Ni1 O21 2.0331(18) .
Ni1 O1W 2.0612(19) .
Ni1 O3W 2.066(2) .
Ni1 O4W 2.0786(17) .
Ni1 O2W 2.0972(19) .
O1W H1WA 0.84000(12) .
O1W H1WB 0.84000(12) .
O2W H2WB 0.84000(12) .
O2W H2WA 0.84000(13) .
O3W H3WA 0.84000(11) .
O3W H3WB 0.84000(13) .
O4W H4WB 0.84000(12) .
O4W H4WA 0.84000(12) .
O5W H5WA 0.8400 .
O5W H5WB 0.8400 .
O6W H6WA 0.8400 .
O6W H6WB 0.8400 .
O13 H13O 0.8200 .
O23 H23O 0.8200 .
