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_7228215
_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         'C70 H54 Cd2 N10 O24, C3 H7 N O, 4(H2 O)'
_chemical_formula_sum            'C73 H69 Cd2 N11 O29'
_chemical_formula_weight         1789.19
_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
_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                66.80(3)
_cell_angle_beta                 88.82(3)
_cell_angle_gamma                78.25(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3020(17)
_cell_length_b                   14.375(3)
_cell_length_c                   17.195(3)
_cell_measurement_reflns_used    34544
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.291
_cell_volume                     1842.6(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34544
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        24.715
_diffrn_reflns_theta_max         24.715
_diffrn_reflns_theta_min         1.291
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 5594 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(6)
_refine_ls_extinction_coef       0.0206(19)
_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   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         12148
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0609P)^2^+4.0538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                11894
_reflns_number_total             12148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           9
_cod_database_code               7228215
_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
 O29-H29A = O29-H29B
 0.82 with sigma of 0.001
 O28-H28A = O28-H28B
 0.82 with sigma of 0.001
 O26-H26A = O26-H26B
 0.82 with sigma of 0.001
 N10-C71
 1.32 with sigma of 0.02
 O24-H24A = O24-H24B
 0.82 with sigma of 0.01
 O27-H27A = O27-H27B
 0.82 with sigma of 0.001
 N9-C66
 1.44 with sigma of 0.001
 H29A-H29B
 1.34 with sigma of 0.04
 H28A-H28B
 1.34 with sigma of 0.04
 H26A-H26B
 1.34 with sigma of 0.04
 H26B-O25_$1
 1.8 with sigma of 0.04
 H26A-O2_$1
 2.2 with sigma of 0.04
 H28A-O8
 2 with sigma of 0.04
 H24A-H24B
 1.34 with sigma of 0.04
 H24A-Cd2
 2.6 with sigma of 0.04
 H27A-H27B
 1.38 with sigma of 0.04
 H27A-O25
 2 with sigma of 0.04
 H27B-O15
 2 with sigma of 0.04
 Cd2-H24A \\sim Cd2-H24B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C73) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O25, N10, C71, C72, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O22, N9, C65, C66, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Rotating group:
 O21(H21A,H21B)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C18(H18), C22(H22), C38(H38)
5.c Me refined with riding coordinates:
 C66(H66A,H66B,H66C)
5.d 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), C65(H65), C68(H68), C71(H71)
5.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C39(H39A,H39B,
 H39C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              48740
_olex2_submission_special_instructions 'No special instructions were received'