Hydrogen adsorption in azolium and metalated N-heterocyclic carbene containing MOFs
Capon, Patrick K.; Burgun, Alexandre; Coghlan, Campbell J.; Crees, Rachel S.; Doonan, Christian J.; Sumby, Christopher J.; CrystEngComm 18 (2016) 7003–; doi:10.1039/C6CE01549B

data_7226346
_publ_section_title
;
 Hydrogen adsorption in azolium and metalated N-heterocyclic carbene
 containing MOFs
;
_journal_issue                   37
_journal_name_full               CrystEngComm
_journal_page_first              7003
_journal_paper_doi               10.1039/C6CE01549B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C40.25 H35.15 Br0.1 Cu2.1 N6.65 O14.45'
_chemical_formula_weight         984.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-08-20 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.475(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7373(16)
_cell_length_b                   17.9433(14)
_cell_length_c                   10.9131(8)
_cell_measurement_reflns_used    3697
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1319
_cell_measurement_theta_min      2.6701
_cell_volume                     4059.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1695
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18655
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_min         2.676
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             2013
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_platon_squeeze_details
;
In order to subtract the contribution from the disordered 
solvent molecules, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 
122, is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to approx 3 DMF molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e). 
;
_refine_diff_density_max         2.579
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.129
_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     284
_refine_ls_number_reflns         5081
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0848P)^2^+14.6135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3863
_reflns_number_total             5081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01549b2.cif
_cod_data_source_block           2Cu
_cod_depositor_comments
'Adding full bibliography for 7226345--7226349.cif.'
_cod_original_formula_sum        'C40.25 H35.15 Br0.10 Cu2.10 N6.65 O14.45'
_cod_database_code               7226346
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.831
_shelxl_version_number           2014/6
_shelx_res_checksum              66657