In situ identification and absolute separation of small molecules by single crystal X-ray diffraction in metal‒organic frameworks
Gao, Heng Ya; Zhang, Le; Yan, Chang Sheng; Meng, Li Na; Li, Jian Qiang; Meng, Pan Pan; Gong, Le Le; Luo, Feng; CrystEngComm 18 (2016) 5429–; doi:10.1039/C6CE01085G

data_7225574
_publ_section_title
;
 In situ identification and absolute separation of small molecules by
 single crystal X-ray diffraction in metal--organic frameworks
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5429
_journal_paper_doi               10.1039/C6CE01085G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C60 H68 Mn3 N10 O18'
_chemical_formula_weight         1382.06
_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-2014/7
_audit_update_record
;
2016-06-06 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                102.276(3)
_cell_angle_beta                 110.249(3)
_cell_angle_gamma                92.234(3)
_cell_formula_units_Z            1
_cell_length_a                   11.3694(7)
_cell_length_b                   12.4390(7)
_cell_length_c                   12.4649(8)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.40
_cell_volume                     1603.84(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20291
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.688
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.8906
_exptl_absorpt_correction_T_min  0.8794
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       Block
_exptl_crystal_F_000             717
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5620
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+2.5968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4849
_reflns_number_total             5620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01085g2.cif
_cod_data_source_block           C3H7OH
_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 7225572--7225575.cif.
;
_cod_database_code               7225574
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              37240