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_7228217
_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         'C102 H88 Cd4 N14 O38'
_chemical_formula_sum            'C102 H88 Cd4 N14 O38'
_chemical_formula_weight         2567.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.674(4)
_cell_length_b                   23.894(5)
_cell_length_c                   14.086(3)
_cell_measurement_reflns_used    105036
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.962
_cell_measurement_theta_min      1.678
_cell_volume                     6285(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    'ShelXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            105036
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.965
_diffrn_reflns_theta_min         1.678
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 5402 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                           It was determined that the voids processed with SQUEEZE contain five water molecules and four DMF molecules.
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         14957
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+2.6677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                13033
_reflns_number_total             14957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           2
_cod_database_code               7228217
_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
 N6-C41
 1.44 with sigma of 0.02
 N6-C42
 1.44 with sigma of 0.02
 O19-H19A = O19-H19B
 0.82 with sigma of 0.01
 C50B-C51B = C51A-C50A = C47A-C48A = C48B-C47B = C49-C48B = C49-C48A = C49-
 C50A = C50B-C49 = N5-C51B = N5-C51A = N5-C47B = N5-C47A
 1.39 with sigma of 0.02
 N7-C45 = N7-C44
 1.44 with sigma of 0.02
 H19A-H19B
 1.4 with sigma of 0.04
 Cd2-H19A
 2.7 with sigma of 0.04
 H19B-Cd2
 2.7 with sigma of 0.04
3. Restrained planarity
 N5, C49, C51B, C47B, C48B, C50B
 with sigma of 0.1
 N5, C49, C51A, C47A, C48A, C50A
 with sigma of 0.1
4. Rigid bond restraints
 N5, C49, C51A, C47A, C48A, C51B, C50A, C47B, C48B, C50B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(C48A) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C50A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Fixed Sof: C47A(0.3) H47A(0.3) C47B(0.7) H47B(0.7) C48A(0.3) H48A(0.3)
 C48B(0.7) H48B(0.7) C50A(0.3) H50A(0.3) C50B(0.7) H50B(0.7) C51A(0.3)
 H51A(0.3) C51B(0.7) H51B(0.7)
7.a Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C22(H22), C32(H32)
7.b Me refined with riding coordinates:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
7.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C16(H16), C20(H20), C26(H26), C30(H30), C35(H35), C39(H39),
 C40(H40), C43(H43), C47A(H47A), C47B(H47B), C48A(H48A), C48B(H48B), C50A(H50A),
  C50B(H50B), C51A(H51A), C51B(H51B)
7.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C23(H23A,H23B,
 H23C), C41(H41A,H41B,H41C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              11913
_shelx_fab_checksum              53653
_olex2_submission_special_instructions 'No special instructions were received'