A robust metallomacrocyclic motif for the formation interpenetrated coordination polymers
Boer, Stephanie A.; Turner, David R.; CrystEngComm 19 (2017) 2402–; doi:10.1039/C7CE00498B

data_7228213
_publ_section_title
;
 A robust metallomacrocyclic motif for the formation interpenetrated
 coordination polymers
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2402
_journal_paper_doi               10.1039/C7CE00498B
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C88 H51 Cd2 N12 O26, C3 H7 N O, H2 O'
_chemical_formula_sum            'C91 H60 Cd2 N13 O28'
_chemical_formula_weight         2008.32
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-13 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                81.85(3)
_cell_angle_beta                 66.46(3)
_cell_angle_gamma                89.84(3)
_cell_formula_units_Z            1
_cell_length_a                   11.947(2)
_cell_length_b                   13.534(3)
_cell_length_c                   14.618(3)
_cell_measurement_reflns_used    27891
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.256
_cell_measurement_theta_min      1.523
_cell_volume                     2141.2(9)
_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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.985
_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     0.7108
_diffrn_reflns_av_R_equivalents  0.1358
_diffrn_reflns_av_unetI/netI     0.1264
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27891
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        23.000
_diffrn_reflns_theta_max         23.259
_diffrn_reflns_theta_min         1.523
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             1017
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.503
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 3085 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.21(3)
_refine_ls_extinction_coef       0.007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1228
_refine_ls_number_reflns         11796
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0900
_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^)+(0.1599P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2242
_refine_ls_wR_factor_ref         0.2444
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.934
_reflns_Friedel_fraction_max     0.933
_reflns_number_gt                9139
_reflns_number_total             11796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           8
_cod_database_code               7228213
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C19-C18
 1.5 with sigma of 0.02
 O20-C59
 1.2 with sigma of 0.02
 O28-H28A = O28-H28B
 0.84 with sigma of 0.001
 C79-C78
 1.39 with sigma of 0.02
 O25-H25A = O25-H25B
 0.84 with sigma of 0.02
 C26-C25
 1.5 with sigma of 0.02
 N13-C90
 1.44 with sigma of 0.02
 O3-C4
 1.2 with sigma of 0.02
 C3-C2
 1.5 with sigma of 0.02
 N13-C91
 1.44 with sigma of 0.02
 N10-C71
 1.4 with sigma of 0.02
 C48-C47
 1.5 with sigma of 0.005
 C32-C24
 1.5 with sigma of 0.02
 C23-C22
 1.5 with sigma of 0.02
 C37-C29
 1.5 with sigma of 0.02
 O26-H26A = O26-H26B
 0.84 with sigma of 0.001
 C51-C50 = C52-C51 = C53-C48
 1.39 with sigma of 0.02
 C56-C55 = C55-C54 = C57-C56
 1.39 with sigma of 0.02
 C11-C10 = C12-C11 = C14-C13 = C15-C14
 1.39 with sigma of 0.02
 H28A-H28B
 1.38 with sigma of 0.04
 H25A-H25B
 1.34 with sigma of 0.04
 H90A-H42_$1
 2.1 with sigma of 0.04
 C91-C90
 2.5 with sigma of 0.04
 H26A-H26B
 1.38 with sigma of 0.04
 H26B-Cd2
 3 with sigma of 0.04
 Cd1-H25A \\sim Cd1-H25B
 with sigma of 0.02
 Cd2-H26A \\sim Cd2-H26B
 with sigma of 0.02
3. Rigid bond restraints
 N5, C41, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O27, N13, C89, C90, C91
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C60, C61, C62, C63, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N9, C65, C66, C67, C68, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C2(H2), C19(H19), C22(H22), C39(H39)
5.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C23(H23A,H23B,H23C), C38(H38A,H38B,H38C), C91(H91A,H91B,H91C)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C13(H13), C14(H14), C27(H27), C28(H28), C33(H33), C34(H34),
 C41(H41), C42(H42), C44(H44), C45(H45), C49(H49), C50(H50), C55(H55), C56(H56),
  C60(H60), C61(H61), C63(H63), C64(H64), C66(H66), C68(H68), C69(H69),
 C73(H73), C74(H74), C79(H79), C80(H80), C84(H84), C85(H85), C87(H87), C88(H88),
  C89(H89)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              42350
_olex2_submission_special_instructions 'No special instructions were received'