The impact of N,N′-ditopic ligand length and geometry on the structures of zinc-based mixed-linker metal‒organic frameworks
Burrows, Andrew D.; Chan, Siobhan; Gee, William J.; Mahon, Mary F.; Richardson, Christopher; Sebestyen, Viorica M.; Turski, Domenyk; Warren, Mark R.; CrystEngComm  (2017) –; doi:10.1039/C7CE01447C

data_7229194
_publ_section_title
;
 The impact of N,N&#x2032;-ditopic ligand length and geometry on the
 structures of zinc-based mixed-linker metal--organic frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01447C
_journal_year                    2017
_chemical_formula_moiety         'C44 H32 N8 O8 Zn2, 1.0(C3 H7 N O)'
_chemical_formula_sum            'C47 H39 N9 O9 Zn2'
_chemical_formula_weight         1004.61
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-06-17 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.762(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.040(6)
_cell_length_b                   29.598(17)
_cell_length_c                   17.153(11)
_cell_measurement_reflns_used    12052
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.0
_cell_volume                     4971(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_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_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29660
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.202
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         8676
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1047P)^2^+6.2198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7182
_reflns_number_total             8676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01447c2.cif
_cod_data_source_block           cpd-4-db592sc3_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7229194
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C45
 1.2 with sigma of 0.005
 C45-C47 \\sim C45-C46
 with sigma of 0.02
 N9-C47 \\sim N9-C46
 with sigma of 0.005
3. Restrained planarity
 C10, C11, C12, C13, C14, C15, C16
 with sigma of 0.1
 C10, C11A, C12A, C13A, C14A, C15, C16A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C11A \\sim C12A \\sim C13A \\sim C14A \\sim C14 \\sim C13 \\sim C12 \\sim C16A
\\sim C16: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.03 and sigma for terminal
atoms of 0.06
Uanis(N9) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.03 and
sigma for terminal atoms of 0.06
Uanis(C10) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16A) \\sim Ueq: with sigma of 0.03 and
sigma for terminal atoms of 0.06
Uanis(C11) = Uanis(C11A)
5. Others
 Fixed Sof: O9(0.5) N9(0.5) C11(0.25) C12(0.25) H12(0.25) C13(0.25) C14(0.25)
 H14(0.25) C16(0.25) H16A(0.25) H16B(0.25) H16C(0.25) C45(0.5) H45(0.5)
 C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5)
 C11A(0.75) C12A(0.75) H12A(0.75) C13A(0.75) C14A(0.75) H14A(0.75) C16A(0.75)
 H16D(0.75) H16E(0.75) H16F(0.75)
6.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C3(H3A), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14),
 C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C12A(H12A), C14A(H14A)
6.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C16A(H16D,H16E,H16F)
;
_shelx_res_checksum              77795
_shelx_fab_checksum              46086