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_7227412
_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         '0.17(C864 H648 Ag36 N144 O36 S72), 5(B1 F4)'
_chemical_formula_sum            'C144 H108 Ag6 B5 F20 N24 O6 S12'
_chemical_formula_weight         3736.71
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_audit_creation_date             2016-06-30
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   26.0470(11)
_cell_length_b                   26.0470(11)
_cell_length_c                   41.751(2)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.79
_cell_measurement_theta_min      2.44
_cell_volume                     24530.9(19)
_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)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41376
_diffrn_reflns_theta_full        30.5243
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5175
_exptl_crystal_description       block
_exptl_crystal_F_000             11184.3315
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.3014
_refine_diff_density_min         -0.7602
_refine_diff_density_rms         0.1926
_refine_ls_d_res_high            0.6997
_refine_ls_d_res_low             9.5092
_refine_ls_goodness_of_fit_ref   1.0586
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8300
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.0559
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0978P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              32
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              59
_reflns_limit_l_min              -59
_reflns_number_gt                5226
_reflns_number_total             8300
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6ce02589g2.cif
_cod_data_source_block           mo_Frankie_MOF_dry1W_0m_a
_cod_depositor_comments
'Adding full bibliography for 7227411--7227413.cif.'
_cod_database_code               7227412
_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
 F3-F4 \\sim F3-F5 \\sim F3-F6 \\sim F4-F5 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.005
 B1-F1 \\sim B2-F3 \\sim B2-F4 \\sim B2-F5 \\sim B2-F6
 with sigma of 0.005
3. Rigid bond restraints
 F1, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.06
 C20, C15
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.006
4. Uiso/Uaniso restraints and constraints
F1 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.003 and sigma
for terminal atoms of 0.06
C20 \\sim C15: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.006
Uanis(B2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Others
 Fixed Sof: F3(0.5) F4(0.5) F5(0.5) F6(0.5) B2(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C12(H12), C14(H14), C18(H18),
 C21(H21), C22(H22), C23(H23), C24(H24)
6.b Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C16(H16a,H16b,H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'