Porous Polyrotaxane Coordination Networks Containing Two Distinct Conformers of a Discontinuously Flexible Ligand.
Hawes, Chris S.; Knowles, Gregory P.; Chaffee, Alan L.; White, Keith F.; Abrahams, Brendan F.; Batten, Stuart R.; Turner, David R.; Inorganic chemistry 55 (2016) 10467–10474; doi:10.1021/acs.inorgchem.6b01713

data_4348836
_publ_section_title
;
 Porous Polyrotaxane Coordination Networks Containing Two Distinct
 Conformers of a Discontinuously Flexible Ligand.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10467
_journal_page_last               10474
_journal_paper_doi               10.1021/acs.inorgchem.6b01713
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C44 H41 N5 O8 Zn2'
_chemical_formula_sum            'C44 H41 N5 O8 Zn2'
_chemical_formula_weight         898.56
_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   geom
_audit_creation_date             2016-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                114.67(3)
_cell_angle_beta                 95.03(3)
_cell_angle_gamma                92.65(3)
_cell_formula_units_Z            2
_cell_length_a                   11.739(2)
_cell_length_b                   13.760(3)
_cell_length_c                   16.428(3)
_cell_measurement_reflns_used    20423
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      0.380
_cell_volume                     2392.0(10)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62638
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.941
_diffrn_reflns_theta_min         1.374
_diffrn_source                   'Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XScale within XDS'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.125
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         11186
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1142P)^2^+2.3579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7766
_reflns_number_total             11186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01713_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4348836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N4-C47
 1.5 with sigma of 0.02
 C47-C46
 1.5 with sigma of 0.02
 C38-C37
 1.45 with sigma of 0.02
 C37-C36
 1.45 with sigma of 0.02
 C36-N6
 1.45 with sigma of 0.02
 N6-C35
 1.45 with sigma of 0.02
 C35-C34
 1.45 with sigma of 0.02
 C26-C27
 1.35 with sigma of 0.02
 C38-N5
 1.45 with sigma of 0.02
 N5-C34
 1.45 with sigma of 0.02
 N5-C25
 1.45 with sigma of 0.02
 C21-C27
 1.35 with sigma of 0.02
 C33-C28 \\sim C29-C28
 with sigma of 0.02
 C27-C21 \\sim C22-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C36) = Uanis(C38) = Uanis(C37) = Uanis(N5) = Uanis(C34) = Uanis(C35) =
Uanis(N6)
Uanis(C23) = Uanis(C30)
Uanis(C27) = Uanis(C33)
Uanis(C26) = Uanis(C32)
4. Rigid body (RIGU) restrains
 C40, C41, C42, C43, C44, C45, C51, C52, C53, C54, C55
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N3, N4, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N5, N6, C34, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C22, C23, C31, C32, C33
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C26, C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C22, C23, C25, C26, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27, C21, C22, C23, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: N3(0.5) N4(0.5) N5(0.5) N6(0.5) C21(0.5) C22(0.5) H22(0.5)
 C23(0.5) H23(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5)
 C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) C32(0.5) H32(0.5) C33(0.5)
 H33(0.5) C34(0.5) H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) C37(0.5) H37A(0.5) H37B(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) C44(0.5) H44(0.5) C45(0.5)
 H45(0.5) C46(0.5) H46A(0.5) H46B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C48(0.5)
 H48A(0.5) H48B(0.5) C49(0.5) H49A(0.5) H49B(0.5) C50(0.5) H50A(0.5) H50B(0.5)
 C51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5)
 H55(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C14(H14), C15(H15), C17(H17), C18(H18),
 C22(H22), C23(H23), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33),
  C41(H41), C42(H42), C44(H44), C45(H45), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61)
;
_shelx_res_checksum              33946
_shelx_hkl_checksum              79601
_shelx_fab_checksum              8503
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'