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_7228216
_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         'C60 H40 N8 O16 Zn2, C0.3 H2.3 O'
_chemical_formula_sum            'C60.3 H42.3 N8 O17 Zn2'
_chemical_formula_weight         1281.66
_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
_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            4
_cell_length_a                   17.345(4)
_cell_length_b                   22.362(5)
_cell_length_c                   13.817(3)
_cell_measurement_reflns_used    89192
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.981
_cell_measurement_theta_min      1.474
_cell_volume                     5359(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 0.988
_diffrn_measured_fraction_theta_max 0.987
_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  0.0855
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            89192
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.984
_diffrn_reflns_theta_min         1.474
_diffrn_source                   'MX1 beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       cube
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.522
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 4819 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         12785
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1289P)^2^+2.7002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1795
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                11756
_reflns_number_total             12785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00498b2.cif
_cod_data_source_block           5
_cod_original_cell_volume        5359.2(19)
_cod_original_formula_sum        'C60.30 H42.30 N8 O17 Zn2'
_cod_database_code               7228216
_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
 C61-O17
 1.4 with sigma of 0.005
 C61-C44_$1
 3.4 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H17(0.7) H17A(0.7) C61(0.3) H61A(0.3) H61B(0.3) H61C(0.3)
5.a Free rotating group:
 O17(H17,H17A)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C18(H18), C22(H22), C38(H38)
5.c Me refined with riding coordinates:
 C39(H39A,H39B,H39C)
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), C46(H46), C47(H47), C49(H49), C50(H50),
  C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60)
5.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              77075
_olex2_submission_special_instructions 'No special instructions were received'