Robust Barium Phosphonate Metal‒Organic Frameworks Synthesized under Aqueous Conditions
Salmeia, Khalifah A.; Dolabella, Simone; Parida, Dambarudhar; Frankcombe, Terry J.; Afaneh, Akef T.; Cordova, Kyle E.; Al-Maythalony, Bassem; Zhao, Shanyu; Civioc, Romain; Marashdeh, Ali; Spingler, Bernhard; Frison, Ruggero; Neels, Antonia; ACS Materials Letters  (2021) 1010–1015; doi:10.1021/acsmaterialslett.1c00275

data_4518816
_publ_section_title
;
 Robust Barium Phosphonate Metal--Organic Frameworks Synthesized under
 Aqueous Conditions
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              1010
_journal_page_last               1015
_journal_paper_doi               10.1021/acsmaterialslett.1c00275
_journal_year                    2021
_chemical_formula_moiety         '0.5(C20 H32 Ba4 N16 O28 P8), 2(H2 O)'
_chemical_formula_sum            'C10 H20 Ba2 N8 O16 P4'
_chemical_formula_weight         906.90
_chemical_name_systematic        C10H18Ba2N8O16P4
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.185(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.0869(11)
_cell_length_b                   13.5308(10)
_cell_length_c                   7.0893(5)
_cell_measurement_reflns_used    11937
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      1.49
_cell_volume                     1310.07(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8343
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.089
_diffrn_reflns_theta_max         25.089
_diffrn_reflns_theta_min         1.491
_exptl_absorpt_coefficient_mu    3.320
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS in PLATON'
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             872
_exptl_crystal_preparation       synthesis
_exptl_crystal_recrystallization_method 'solvent evaporation'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.907
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.0021(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2335
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0619P)^2^+0.3699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2168
_reflns_number_total             2335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tz1c00275_si_003.cif
_cod_data_source_block           ba-mof-4-5
_cod_database_code               4518816
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.491
_shelx_estimated_absorpt_t_min   0.288
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O2W-H2WB
 0.84 with sigma of 0.01
 H1WA-H1WB = H2WA-H2WB
 1.34 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
3.b Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5)
;
_shelx_res_checksum              84883
_shelx_hkl_checksum              34387
_olex2_exptl_crystal_mounting_method 'was mounted'
_olex2_submission_original_sample_id Ba-MOF-4-5
_olex2_submission_special_instructions 'No special instructions were received'