Compositional control of pore geometry in multivariate metal-organic frameworks: an experimental and computational study.
Cadman, Laura K.; Bristow, Jessica K.; Stubbs, Naomi E.; Tiana, Davide; Mahon, Mary F.; Walsh, Aron; Burrows, Andrew D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4316–4326; doi:10.1039/c5dt04045k

data_7037660
_publ_section_title
;
 Compositional control of pore geometry in multivariate metal-organic
 frameworks: an experimental and computational study.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4316
_journal_page_last               4326
_journal_paper_doi               10.1039/c5dt04045k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '0.25(C88 H48 N9.6 O32 Zn8)'
_chemical_formula_sum            'C29.8 H38.6 N5 O10.6 Zn2'
_chemical_formula_weight         767.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c'
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-13 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9813(3)
_cell_length_b                   14.9813(3)
_cell_length_c                   19.2011(6)
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.4540
_cell_measurement_theta_min      4.6060
_cell_volume                     4309.48(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14611
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.930
_diffrn_reflns_theta_min         5.473
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
_exptl_special_details 
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1589
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.099
_refine_diff_density_max         2.067
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2088
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0650
_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^)+(0.1386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1489
_reflns_number_total             2088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04045k2.cif
_cod_data_source_block           s14adb5_sq
_cod_depositor_comments
'Adding full bibliography for 7037655--7037663.cif.'
_cod_original_cell_volume        4309.5(2)
_cod_original_formula_sum        'C29.80 H38.60 N5 O10.60 Zn2'
_cod_database_code               7037660
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 N3A-C6 = N3-C5
 1.38 with sigma of 0.02
 N3A-C4 \\sim N3A-C5_$1 \\sim N3-C4 \\sim N3-C6_$1
 with sigma of 0.005
3. Restrained planarity
 C3, C4, C5, C6, N3, N3A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of 0.015 and sigma
for terminal atoms of 0.01
5. Others
 Fixed Sof: C10(0.375) H10A(0.375) H10B(0.375) C7(0.375) H7A(0.375) H7B(0.375)
 C9(0.375) H9A(0.375) H9B(0.375) C8(0.375) H8A(0.375) H8B(0.375) N3A(0.065)
 N3(0.035)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C7(H7A,H7B), C9(H9A,H9B), C8(H8A,H8B)
;
_shelx_fab_checksum              6428
_olex2_submission_special_instructions 'No special instructions were received'