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_7228219
_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 H48 Cd2 N12 O24'
_chemical_formula_sum            'C88 H48 Cd2 N12 O24'
_chemical_formula_weight         1882.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 107.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.369(3)
_cell_length_b                   17.967(4)
_cell_length_c                   18.470(4)
_cell_measurement_reflns_used    121534
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.894
_cell_measurement_theta_min      1.159
_cell_volume                     4852(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            121534
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.897
_diffrn_reflns_theta_min         1.159
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 8712 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                          The crystals of 7 could not be obtained phase pure, so it is not possible to determine the exact solvent composition in the pores. However as each assymetric unit contains a void filled with 162 or 163 electrons, this can be equated to 4 DMF molecules (160 electrons) per asymmetric unit. 
;
_refine_ls_abs_structure_Flack   0.082(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         22959
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+1.5722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                19973
_reflns_number_total             22959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           7
_cod_original_cell_volume        4851.6(19)
_cod_database_code               7228219
_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
2. Restrained distances
 C10-C18
 1.48 with sigma of 0.02
 C30-C38
 1.48 with sigma of 0.01
 C20-C19 = C21-C19
 1.5 with sigma of 0.005
3. Rigid bond restraints
 N9, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, N6, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C47, C48, C49, C50, C51, C52, C53, C54, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N8, C61, C62, C63, C64, C65
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C87) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C2(H2), C19(H19), C23(H23), C39(H39)
5.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C14(H14), C15(H15), C28(H28), C29(H29), C34(H34), C35(H35),
 C42(H42), C43(H43), C45(H45), C46(H46), C50(H50), C51(H51), C56(H56), C57(H57),
  C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C69(H69),
 C70(H70), C74(H74), C75(H75), C80(H80), C82(H82), C86(H86), C87(H87), C89(H89),
  C90(H90)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C24(H24A,H24B,H24C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              47539
_shelx_fab_checksum              87283
_olex2_submission_special_instructions 'No special instructions were received'