Structural characterization of framework‒gas interactions in the metal‒organic framework Co2(dobdc) by in situ single-crystal X-ray diffraction
Gonzalez, Miguel; Mason, Jarad; Bloch, Eric D.; Teat, Simon; Gagnon, Kevin J.; Morrison, Gregory Y.; Queen, Wendy Lee; Long, Jeffrey R.; Chem. Sci.  (2017) –; doi:10.1039/C7SC00449D

data_1545766
_publ_section_title
;
 Structural characterization of framework--gas interactions in the
 metal--organic framework Co2(dobdc) by in situ single-crystal X-ray
 diffraction
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC00449D
_journal_year                    2017
_chemical_formula_moiety         '(C8 H2 Co2 O4), 1.32(P4)'
_chemical_formula_sum            'C8 H2 Co2 O6 P5.28'
_chemical_formula_weight         475.58
_chemical_name_common            Co2(dobdc)(P4)1.32
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3368 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-01-28 deposited with the CCDC.
2017-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.7348(8)
_cell_length_b                   25.7348(8)
_cell_length_c                   6.8385(2)
_cell_measurement_reflns_used    9311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.233
_cell_measurement_theta_min      3.397
_cell_volume                     3922.2(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43953
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         37.238
_diffrn_reflns_theta_min         3.398
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.034
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0760 before and 0.0473 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0758 before and 0.0462 after correction.
 The Ratio of minimum to maximum transmission is 0.85.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 43953 reflections, Rint = 0.0392
 (30737 with I > 3sig(I), Rint = 0.0342)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2081
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.388
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3479
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0822
_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^)+(0.1256P)^2^+39.0610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3064
_reflns_number_total             3479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00449d2.cif
_cod_data_source_block           Co2dobdc-P4
_cod_original_cell_volume        3922.2(3)
_cod_database_code               1545766
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.611
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.479(4) 0.521(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 P1A-P2A \\sim P1A-P3A \\sim P1A-P4A \\sim P1B-P2B \\sim P1B-P3B \\sim P1B-P4B
\\sim P2A-P3A \\sim P2A-P4A
 \\sim P3A-P4A \\sim P2B-P3B \\sim P2B-P4B \\sim P3B-P4B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
P1A \\sim P3A \\sim P4A \\sim P2A \\sim P1B \\sim P3B \\sim P4B \\sim P2B:
within 2.3A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 P1A, P3A, P4A, P2A, P1B, P3B, P4B, P2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(P1A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=FVAR(1)
 Sof(P1B)=Sof(P2B)=Sof(P3B)=Sof(P4B)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_checksum              66035
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'