Rational Synthesis of Mixed-Metal Microporous Metal‒Organic Frameworks with Controlled Composition Using Mechanochemistry
Ayoub, Ghada; Karadeniz, Bahar; Howarth, Ashlee J.; Farha, Omar K.; Đilović, Ivica; Germann, Luzia S.; Dinnebier, Robert E.; Užarević, Krunoslav; Friščić, Tomislav; Chemistry of Materials 31 (2019) 5494–; doi:10.1021/acs.chemmater.9b01068

data_4003046
_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       '\w 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/[\s^2^(Fo^2^)+(0.0852P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_res_checksum              27067
_shelx_hkl_checksum              50572