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_7037662
_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         '0.5(C44 H24 Br2.8 I1.2 N4 O16 Zn4)'
_chemical_formula_sum            'C29.8 H36.2 Br1.4 I0.6 N4.6 O10.6 Zn2'
_chemical_formula_weight         947.19
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2b 2bc'
_space_group_name_H-M_alt        'P n c b'
_symmetry_space_group_name_Hall  '-P 2b 2bc'
_symmetry_space_group_name_H-M   'P n c b :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            2
_cell_length_a                   9.6270(3)
_cell_length_b                   13.2670(4)
_cell_length_c                   17.2190(5)
_cell_measurement_reflns_used    41558
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2199.23(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_laue_measured_fraction_full 0.979
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31992
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         3.527
_exptl_absorpt_coefficient_mu    2.834
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1953
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0950
_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^)+(0.1353P)^2^+15.3650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2457
_refine_ls_wR_factor_ref         0.2667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1559
_reflns_number_total             1953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04045k2.cif
_cod_data_source_block           k14adb2
_cod_depositor_comments
'Adding full bibliography for 7037655--7037663.cif.'
_cod_original_cell_volume        2199.24(11)
_cod_original_formula_sum        'C29.80 H36.20 Br1.40 I0.60 N4.60 O10.60 Zn2'
_cod_database_code               7037662
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.281
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C2-C3A = C2-C3B = C2-C4A = C2-C4B
 1.4 with sigma of 0.005
 C3A-C4A_$1
 1.4 with sigma of 0.005
 C4B-C3B_$1
 1.4 with sigma of 0.005
 C3A-I1A \\sim C4A-I1B
 with sigma of 0.005
 C3B-Br1A \\sim C4B-Br1B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Br1A \\sim I1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Br1B \\sim I1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C3A) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C4B)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I1A) \\sim Ueq, Uanis(I1B) \\sim Ueq, Uanis(Br1B) \\sim Ueq, Uanis(Br1A)
\\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(C4A) = Uanis(C4B)
Uanis(C3A) = Uanis(C3B)
Uanis(Br1A) = Uanis(I1A)
4. Others
 Fixed Sof: I1A(0.12) I1B(0.03) Br1A(0.3) Br1B(0.05) C5(0.5) H5A(0.5) H5B(0.5)
 C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C3A(0.65) C4A(0.65)
 C3B(0.35) C4B(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
;
_olex2_submission_special_instructions 'No special instructions were received'