Second-order programming the synthesis of metal-organic frameworks.
Fishburn, Mitchell G.; Skelton, Dayne R.; Telfer, Shane G.; Wagner, Pawel; Richardson, Christopher; Chemical communications (Cambridge, England) 56 (2020) 12355–12358; doi:10.1039/d0cc05451h

data_7127208
_publ_section_title
;
 Second-order programming the synthesis of metal-organic frameworks.
;
_journal_issue                   82
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12355
_journal_page_last               12358
_journal_paper_doi               10.1039/d0cc05451h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C35 H30 N4 O8'
_chemical_formula_sum            'C35 H30 N4 O8'
_chemical_formula_weight         634.63
_chemical_name_systematic
'Dimethyl 2-(((1-(4,4'-bis(methoxycarbonyl)-[1,1'-biphenyl]-2-yl)-1H-1,2,3-triazol-4-yl)methyl)amino)-[1,1'-biphenyl]-4,4'-dicarboxylate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-06 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                94.515(2)
_cell_angle_beta                 101.132(2)
_cell_angle_gamma                96.424(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5406(3)
_cell_length_b                   10.8847(2)
_cell_length_c                   13.6301(4)
_cell_measurement_reflns_used    27521
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      30.2840
_cell_measurement_theta_min      2.2360
_cell_volume                     1516.65(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(1)
_diffrn_detector                 'HyPix Bantam HPC 3000'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-141.53  368
  2  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 137.28  368
  3  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00  60.00  368
  4  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 -30.00  368
  5  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-102.91  368
  6  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00   0.00  368
  7  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00   0.00  368
  8  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-180.00  368
  9  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00  30.00  368
 10  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-150.00  368
 11  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 -60.00  368
 12  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 120.00  368
 13  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 -16.66  368
 14  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00-124.70  368
 15  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 -90.00  368
 16  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00  82.70  368
 17  \w    -74.00  16.00   0.50   10.00    --   20.00  54.00 150.00  180
 18  \w    -74.00 110.00   0.50   10.00    --   20.00  54.00 105.01  368
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (Paciorek et al (1999). Acta A55, 543-557)'
_diffrn_orient_matrix_UB_11      0.0191132000
_diffrn_orient_matrix_UB_12      -0.0531877000
_diffrn_orient_matrix_UB_13      -0.0238412000
_diffrn_orient_matrix_UB_21      0.0333206000
_diffrn_orient_matrix_UB_22      0.0385422000
_diffrn_orient_matrix_UB_23      -0.0290568000
_diffrn_orient_matrix_UB_31      0.0575222000
_diffrn_orient_matrix_UB_32      0.0056466000
_diffrn_orient_matrix_UB_33      0.0378199000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79549
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.247
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018) 
Analytical numeric absorption correction using a multifaceted crystal model
 based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897). 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       'faceted block'
_exptl_crystal_F_000             664
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol / dichloromethane'
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.201
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0600P)^2^+0.2874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5927
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05451h3.cif
_cod_data_source_block           exp_197_mf2
_cod_depositor_comments
'Adding full bibliography for 7127207--7127208.cif.'
_cod_database_code               7127208
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C35 H30 N4 O8'
_chemical_oxdiff_usercomment     'Triazole recollection in 40.47a'
_diffrn_oxdiff_digest_frames
;
018d9513798eabc009664e598c164744d306436010f
;
_diffrn_oxdiff_digest_hkl
;
01a066a2cbc48b75db1b9deb1b24896839d75f
;
_reflns_odcompleteness_completeness 98.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C20(H20),
 C25(H25), C26(H26), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              5195
_olex2_exptl_crystal_mounting_method 'Mitegen mount + Paratone'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.949