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_7226348
_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            'C72.25 H50.25 Br1.2 Cu1.2 N10.55 O26.15 Zn4'
_chemical_formula_weight         1918.20
_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
;
2016-08-15 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.889(4)
_cell_length_b                   18.004(4)
_cell_length_c                   10.913(2)
_cell_measurement_reflns_used    5725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.64
_cell_measurement_theta_min      0.71
_cell_volume                     4103.1(14)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41452
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.085
_diffrn_reflns_theta_min         1.493
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             1927
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.676
_exptl_transmission_factor_min   0.619
_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 60, 
is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to approx 1.5 DMF molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e). 
;
_refine_diff_density_max         4.567
_refine_diff_density_min         -4.015
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5725
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0760
_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^)+(0.1053P)^2^+54.0311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5509
_reflns_number_total             5725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01549b2.cif
_cod_data_source_block           1-Cu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7226345--7226349.cif.
;
_cod_original_formula_sum
'C72.25 H50.25 Br1.20 Cu1.20 N10.55 O26.15 Zn4'
_cod_database_code               7226348
_shelxl_version_number           2014/6
_shelx_res_checksum              37851