Computational and Experimental Assessment of CO2 Uptake in Phosphonate Monoester Metal‒Organic Frameworks
Gelfand, Benjamin S.; Huynh, Racheal P. S.; Collins, Sean P.; Woo, Tom K.; Shimizu, George K. H.; Chemistry of Materials 29 (2017) 10469–; doi:10.1021/acs.chemmater.7b04108

data_4002878
_publ_section_title
;
 Computational and Experimental Assessment of CO2 Uptake in Phosphonate
 Monoester Metal--Organic Frameworks
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              10469
_journal_paper_doi               10.1021/acs.chemmater.7b04108
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety         'C56 H52 Cu3 O18 P6	'
_chemical_formula_sum            'C56 H52 Cu3 O18 P6'
_chemical_formula_weight         1389.45
_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   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                83.882(1)
_cell_angle_beta                 85.728(1)
_cell_angle_gamma                82.705(2)
_cell_formula_units_Z            1
_cell_length_a                   5.0813(1)
_cell_length_b                   15.1585(3)
_cell_length_c                   29.3246(7)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2223.42(8)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.842
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2156
_diffrn_reflns_Laue_measured_fraction_full 0.842
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7376
_diffrn_reflns_point_group_measured_fraction_full 0.842
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         5.114
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M., SADABS 1997'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             709
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
The SQUEEZE routine of the program PLATON was used

in order to eliminate the contribution of disordered solvents molecules,

thereby a final model based only on the ordered part of the crystal structure

was obtained.

The SQUEEZE routine suggested that

a total potential solvent area volume of 955.0Ang^3^[43.0% of cell volume],

and a void electron population of 47 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.

[R values before SQUEEZE]

R1 = 0.0840, wR2 = 0.1620 for >2sigma(I) data

R1 = 0.1710, wR2 = 0.1903, GooF = S = 1.105 for all data

( 23883 data and 913 restraint / 1438 parameters)

;
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7376
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3758
_reflns_number_total             7376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b04108_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4002878--4002879.cif.'
_cod_database_code               4002878
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014/6
_shelx_res_checksum              12722
_shelx_hkl_checksum              71204