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_7127207
_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         'C51 H33 N3 O13 Zn4'
_chemical_formula_sum            'C51 H33 N3 O13 Zn4'
_chemical_formula_weight         1157.28
_chemical_name_common            WUF-52
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           113
_space_group_name_Hall           'P -4 2ab'
_space_group_name_H-M_alt        'P -4 21 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   geom
_audit_creation_date             2020-08-06
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2000(12)
_cell_length_b                   17.2000(12)
_cell_length_c                   17.2000(12)
_cell_measurement_reflns_used    6446
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      58.900
_cell_measurement_theta_min      5.752
_cell_volume                     5088.4(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)
;
_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      292
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
scan:
	Number of images: 56
	           Slice: 20.0000 - 160.0000
	     Image width: 2.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 44
	           Slice: 102.0000 - 212.0000
	     Image width: 2.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 0.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 56
	           Slice: 20.0000 - 160.0000
	     Image width: 2.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 30.0000
	             Phi: 90.0000
	             XTD: 127.4000
	          2theta: 0.0000
scan:
	Number of images: 44
	           Slice: 102.0000 - 212.0000
	     Image width: 2.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 30.0000
	             Phi: 180.0000
	             XTD: 127.4000
	          2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      -0.022675
_diffrn_orient_matrix_UB_12      0.053530
_diffrn_orient_matrix_UB_13      -0.000134
_diffrn_orient_matrix_UB_21      0.013722
_diffrn_orient_matrix_UB_22      0.005672
_diffrn_orient_matrix_UB_23      -0.056207
_diffrn_orient_matrix_UB_31      -0.051742
_diffrn_orient_matrix_UB_32      -0.021954
_diffrn_orient_matrix_UB_33      -0.014848
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2457
_diffrn_reflns_av_unetI/netI     0.1933
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28491
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        58.900
_diffrn_reflns_theta_max         58.900
_diffrn_reflns_theta_min         5.752
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR; Higashi, 1995'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    0.755
_exptl_crystal_description       chip
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 829 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.37(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3824
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.1015
_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^)+(0.1179P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2487
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2884
_reflns_number_total             3824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05451h3.cif
_cod_data_source_block           WUF-52(ds1-83-1p-42(1)m)
_cod_depositor_comments
'Adding full bibliography for 7127207--7127208.cif.'
_cod_original_cell_volume        5088.4(8)
_cod_database_code               7127207
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.426(9)
 0.271(6) 0.303(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N14-C12
 1.4 with sigma of 0.01
 N29-C27
 1.4 with sigma of 0.01
 C27-C30
 2.4 with sigma of 0.04
4. Restrained planarity
 C25, C26, C27, C28
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C15 \\sim
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C24 \\sim
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C30 \\sim C31 \\sim C32 \\sim O1 \\sim
O4 \\sim O5 \\sim O6 \\sim O23: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Same fragment restrains
{C7, C8, C9, C10, C11} sigma for 1-2: 0.001, 1-3: 0.02
as
{C18, C19, C20, C21, C22}
{C7, C8, C9, C10, C11} sigma for 1-2: 0.001, 1-3: 0.02
as
{C24, C25, C26, C27, C28}
7. Others
 Fixed Sof: H12(0.5) N14(0.5) H14(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5)
 C17(0.5) H17(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) N29(0.25) H29(0.25)
 C30(0.25) H30A(0.25) H30B(0.25) C31(0.25) C32(0.25) H32(0.25) H27(0.25)
 Fixed Uiso: N14(0.2) H14(0.2) C15(0.2) H15A(0.2) H15B(0.2) C16(0.2) C17(0.2)
 H17(0.2) N29(0.2) H29(0.2) C30(0.2) H30A(0.2) H30B(0.2) C31(0.2) C32(0.2)
 H32(0.2) H27(0.2)
 Fixed X: N14(0.61565) H14(0.61675) C15(0.63145) H15A(0.68515) H15B(0.627201)
 C16(0.58531) C17(0.550261) H17(0.523101) N29(0.607) H29(0.61275) C30(0.577649)
 H30A(0.56563) H30B(0.52763) C31(0.60381) C32(0.6386) H32(0.66555) H27(0.587)
 Fixed Y: N14(0.544479) H14(0.495449) C15(0.561151) H15A(0.54719)
 H15B(0.61695) C16(0.525391) C17(0.49154) H17(0.46531) N29(1.107) H29(1.101181)
 C30(1.18115) H30A(1.202769) H30B(1.16989) C31(1.24588) C32(1.29707)
 H32(1.336729) H27(1.087)
 Fixed Z: N14(0.702489) H14(0.69274) C15(0.78092) H15A(0.79102) H15B(0.78786)
 C16(0.83782) C17(0.88778) H17(0.926489) N29(1.158001) H29(1.10867)
 C30(1.17584) H30A(1.125161) H30B(1.199321) C31(1.21794) C32(1.25018)
 H32(1.275169) H27(1.16973)
8.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C20(H20), C21(H21), C26(H26)
8.b Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13)
;
_shelx_res_checksum              14177
_olex2_submission_special_instructions 'No special instructions were received'