Ligand Excess "Inverse-Defected" Zr<sub>6</sub> Tetrahedral Tetracarboxylate Framework and Its Thermal Transformation.
Nateghi, Bahareh; Domasevitch, Kostiantyn V.; Bulánek, Roman; Janiak, Christoph; Boldog, Ishtvan; Inorganic chemistry 58 (2019) 12786–12797; doi:10.1021/acs.inorgchem.9b01721

data_4345991
_publ_section_title
;
 Ligand Excess &quot;Inverse-Defected&quot; Zr<sub>6</sub> Tetrahedral
 Tetracarboxylate Framework and Its Thermal Transformation.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12786
_journal_page_last               12797
_journal_paper_doi               10.1021/acs.inorgchem.9b01721
_journal_volume                  58
_journal_year                    2019
_chemical_formula_moiety
;
(Zr 4+)6, C28H29O8 4-, (C28H29O8 3-)2, (O 2-)4, (O H -)6, 2(H2 O), 
6(C3 H7 N O) 
;
_chemical_formula_sum            'C132 H138 N6 O42 Zr6'
_chemical_formula_weight         3027.91
_chemical_name_common
;
coordination-polymeric hexazirconium heptahydroxo pentaaqua complex 
with two anions of tetra-1,3,5,7-(carboxyphenyl)adamantane, 
solvate with N,N-dimethylformamide, formic acid and water
;
_chemical_name_systematic
;
poly{[\m~8~-((adamantane-1,3,5,7-tetrayl)tetra(phen-4-yl))tetra(carboxylate-\
\k<i>O:</i>\k<i>O'</i>)][bis(\m~6~-((adamantane-1,3,5,7-\
tetrayl)tetra(phen-4-yl))(tri(carboxylate-\
\k<i>O:</i>\k<i>O')</i>)(carboxylic acid))]
tetra(\m~3~-oxo)tetra(\m~3~-hydroxido)di(hydroxido)tetraaquahexazirconium(IV)},
solvate with N,N-dimethylformamide, formic acid and water
;
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 101.9120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2611(2)
_cell_length_b                   30.9669(4)
_cell_length_c                   25.4544(3)
_cell_measurement_reflns_used    56519
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      69.11
_cell_measurement_theta_min      3.16
_cell_volume                     18711.8(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)
;
_computing_data_reduction
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;
_computing_molecular_graphics    'Diamond 3.2i (Putz, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
; 
2647 frames, detector distance = 60 mm
;
_diffrn_measurement_device_type  'Stoe Stadivary diffractometer'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            96177
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.929
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.165
_exptl_absorpt_correction_T_max  0.6705
_exptl_absorpt_correction_T_min  0.4922
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       prism
_exptl_crystal_F_000             6056
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         17064
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0627
_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/[\s^2^(Fo^2^)+(0.1681P)^2^+11.2814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14265
_reflns_number_total             17064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic9b01721_si_002.cif
_cod_data_source_block           1_I-HCOOH-no-squeeze
_cod_database_code               4345991
_shelxl_version_number           2014-3