Control of metallo-supramolecular assemblies via steric, hydrogen bonding and argentophilic interactions; formation of a 3-dimensional polymer of circular helicates
Bullock, Samantha J.; Davidson, Francesca S.; Faulkner, Robert A.; Parkes, Gareth M. B.; Rice, Craig R.; Towns-Andrews, Liz; CrystEngComm 19 (2017) 1273–; doi:10.1039/C6CE02589G

data_7227411
_publ_section_title
;
 Control of metallo-supramolecular assemblies via steric, hydrogen bonding
 and argentophilic interactions; formation of a 3-dimensional polymer of
 circular helicates
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1273
_journal_paper_doi               10.1039/C6CE02589G
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety
'2(C62 H48 Ag2 N8 O2 S4), 4(B F4), 3(C H3 N O2)'
_chemical_formula_sum            'C127 H105 Ag4 B4 F16 N19 O10 S8'
_chemical_formula_weight         3092.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-27 deposited with the CCDC.
2017-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                80.419(16)
_cell_angle_beta                 82.135(19)
_cell_angle_gamma                83.58(3)
_cell_formula_units_Z            1
_cell_length_a                   7.820(4)
_cell_length_b                   18.768(9)
_cell_length_c                   25.836(12)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.21
_cell_volume                     3688(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9858
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            101583
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3922
_exptl_crystal_description       needle
_exptl_crystal_F_000             1558.2310
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.7923
_refine_diff_density_min         -1.4445
_refine_diff_density_rms         0.2047
_refine_ls_d_res_high            0.7457
_refine_ls_d_res_low             11.2645
_refine_ls_goodness_of_fit_ref   1.0362
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     887
_refine_ls_number_reflns         18381
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.0319
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.0041
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+5.5763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              25
_reflns_limit_k_min              -24
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                12568
_reflns_number_total             18381
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6ce02589g2.cif
_cod_data_source_block           mo_Rob_EtPh_5_0m
_cod_depositor_comments
'Adding full bibliography for 7227411--7227413.cif.'
_cod_database_code               7227411
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F0aa-B14 \\sim F1-B14 \\sim F12-B14 \\sim F2-B14 \\sim F5-B14 \\sim F10-B14
 with sigma of 0.005
3. Rigid bond restraints
 F0aa, F1, F2, F5, F10, F12
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 O2, C7, O8, N9, O1
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C57, C72, C73, C80, C88
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C14, C36, C79, C94, C97
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C21, C26, C81
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
 C69, C62
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
4. Uiso/Uaniso restraints and constraints
F0aa \\sim F1 \\sim F2 \\sim F5 \\sim F10 \\sim F12: within 2A with sigma of
0.003 and sigma for terminal atoms of 0.006
O2 \\sim C7 \\sim H \\sim Ha \\sim Hb \\sim O8 \\sim N9 \\sim O1: within 2A
with sigma of 0.003 and sigma for terminal atoms of 0.006
C57 \\sim C72 \\sim C73 \\sim C80 \\sim C88: within 2A with sigma of 0.003 and
sigma for terminal atoms of 0.006
C14 \\sim C36 \\sim C79 \\sim C94 \\sim C97: within 2A with sigma of 0.003 and
sigma for terminal atoms of 0.006
C21 \\sim C26 \\sim C81: within 2A with sigma of 0.003 and sigma for terminal
atoms of 0.006
C69 \\sim C62: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F2)=Sof(F10)=1-FVAR(1)
 Sof(F5)=Sof(F12)=FVAR(1)
 Fixed Sof: C7(0.5) H(0.5) Ha(0.5) Hb(0.5) O8(0.5) N9(0.5) O1(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C26(H26a,H26b), C38(H38a,H38b), C57(H57a,H57b), C81(H81a,H81b)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C18(H18), C22(H22), C24(H24), C27(H27), C29(H29),
 C31(H31), C39(H39), C44(H44), C46(H46), C49(H49), C52(H52), C55(H55), C56(H56),
  C59(H59), C61(H61), C63(H63), C65(H65), C66(H66), C68(H68), C71(H71),
 C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C79(H79), C80(H80), C84(H84),
  C88(H88), C90(H90), C94(H94), C97(H97)
6.c Idealised Me refined as rotating group:
 C34(H34a,H34b,H34c), C62(H62a,H62b,H62c), C7(H,Ha,Hb), C10(Hc,Hd,He)
;
_olex2_submission_special_instructions 'No special instructions were received'