Solvent-vapour-assisted pathways and the role of pre-organization in solid-state transformations of coordination polymers
Wright, James S.; Vitórica-Yrezábal, Iñigo J.; Adams, Harry; Thompson, Stephen P.; Hill, Adrian H.; Brammer, Lee; IUCrJ 2 (2015) 188–197; doi:10.1107/S2052252515000147

data_1542775
_publ_section_title
;
 Solvent-vapour-assisted pathways and the role of pre-organization in
 solid-state transformations of coordination polymers
;
_journal_issue                   2
_journal_name_full               IUCrJ
_journal_page_first              188
_journal_page_last               197
_journal_paper_doi               10.1107/S2052252515000147
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         'C8 H10, C20 H8 Ag2 F13 N2 O4, F'
_chemical_formula_sum            'C28 H18 Ag2 F14 N2 O4'
_chemical_formula_weight         928.18
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.472(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3750(6)
_cell_length_b                   22.5963(10)
_cell_length_c                   13.3460(7)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.45
_cell_volume                     3146.5(3)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25586
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         1.892
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1011 before and 0.0786 after correction.
The Ratio of minimum to maximum transmission is 0.8102.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.959
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.828
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7203
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0599P)^2^+35.1346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6202
_reflns_number_total             7203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bi5040.cif
_cod_data_source_block           1-mxyl
_cod_database_code               1542775
_publcif_datablock.id            {5aa61258-3b20-483e-9b99-3ea75f66a2ee}
_shelxl_version_number           2013-4
_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. Shared sites
{F4Z, F4B}
3. Restrained distances
 C1-C2
 1.54 with sigma of 0.001
 C2-C3
 1.54 with sigma of 0.001
 C3-C4
 1.54 with sigma of 0.001
 C1-C2'
 1.54 with sigma of 0.001
 C2'-C3'
 1.54 with sigma of 0.001
 C3'-C4'
 1.54 with sigma of 0.001
 C2-F2A
 1.35 with sigma of 0.001
 C2-F2B
 1.35 with sigma of 0.001
 C3-F3A
 1.35 with sigma of 0.001
 C3-F3B
 1.35 with sigma of 0.001
 C4-F4A
 1.35 with sigma of 0.001
 C4-F4B
 1.35 with sigma of 0.001
 C4-F4C
 1.35 with sigma of 0.001
 C2'-F2Z
 1.35 with sigma of 0.001
 C2'-F2Y
 1.35 with sigma of 0.001
 C3'-F3Z
 1.35 with sigma of 0.001
 C3'-F3Y
 1.35 with sigma of 0.001
 C4'-F4X
 1.35 with sigma of 0.001
 C4'-F4Y
 1.35 with sigma of 0.001
 C4'-F4Z
 1.35 with sigma of 0.001
 F2A-F2B
 2.16 with sigma of 0.001
 F3A-F3B
 2.16 with sigma of 0.001
 F4A-F4B
 2.16 with sigma of 0.001
 F4B-F4C
 2.16 with sigma of 0.001
 F2Z-F2Y
 2.16 with sigma of 0.001
 F3Z-F3Y
 2.16 with sigma of 0.001
 F4X-F4Y
 2.16 with sigma of 0.001
 F4Y-F4Z
 2.16 with sigma of 0.001
 C2-C4
 2.6 with sigma of 0.001
 C2'-C4'
 2.6 with sigma of 0.001
 C11-C12
 1.54 with sigma of 0.001
 C12-C13
 1.54 with sigma of 0.001
 C13-C14
 1.54 with sigma of 0.001
 C11-C12'
 1.54 with sigma of 0.001
 C12'-C13'
 1.54 with sigma of 0.001
 C13'-C14'
 1.54 with sigma of 0.001
 C12-F12A
 1.35 with sigma of 0.001
 C12-F12B
 1.35 with sigma of 0.001
 C13-F13A
 1.35 with sigma of 0.001
 C13-F13B
 1.35 with sigma of 0.001
 C14-F14A
 1.35 with sigma of 0.001
 C14-F14B
 1.35 with sigma of 0.001
 C14-F14C
 1.35 with sigma of 0.001
 C12'-F12Z
 1.35 with sigma of 0.001
 C12'-F12Y
 1.35 with sigma of 0.001
 C13'-F13Z
 1.35 with sigma of 0.001
 C13'-F13Y
 1.35 with sigma of 0.001
 C14'-F14X
 1.35 with sigma of 0.001
 C14'-F14Y
 1.35 with sigma of 0.001
 C14'-F14Z
 1.35 with sigma of 0.001
 F12A-F12B
 2.16 with sigma of 0.001
 F13A-F13B
 2.16 with sigma of 0.001
 F14A-F14B
 2.16 with sigma of 0.001
 F14B-F14C
 2.16 with sigma of 0.001
 F12Z-F12Y
 2.16 with sigma of 0.001
 F13Z-F13Y
 2.16 with sigma of 0.001
 F14X-F14Y
 2.16 with sigma of 0.001
 F14Y-F14Z
 2.16 with sigma of 0.001
 C12-C14
 2.6 with sigma of 0.001
 C12'-C14'
 2.6 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C2 \\sim C2': within 1.7A with sigma of 0.003 and sigma for terminal atoms of
0.006
F4Z \\sim C4' \\sim F4X \\sim F4Y \\sim C3' \\sim F3Y \\sim F3Z \\sim C2' \\sim
F2Y \\sim F2Z: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uiso(F4Z) = Uiso(F4B)
5. Others
 Sof(C12')=Sof(F12Y)=Sof(F12Z)=Sof(C13')=Sof(F13Y)=Sof(F13Z)=Sof(C14')=
 Sof(F14X)=Sof(F14Y)=Sof(F14Z)=1-FVAR(1)
 Sof(C12)=Sof(F12A)=Sof(F12B)=Sof(C13)=Sof(F13A)=Sof(F13B)=Sof(C14)=Sof(F14A)=
 Sof(F14B)=Sof(F14C)=FVAR(1)
 Sof(C2')=Sof(F2Z)=Sof(F2Y)=Sof(C3')=Sof(F3Y)=Sof(F3Z)=Sof(C4')=Sof(F4X)=
 Sof(F4Y)=Sof(F4Z)=1-FVAR(2)
 Sof(C2)=Sof(F2A)=Sof(F2B)=Sof(C3)=Sof(F3A)=Sof(F3B)=Sof(C4)=Sof(F4A)=Sof(F4B)=
 Sof(F4C)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C50(H50), C51(H51), C53(H53), C55(H55), C100(H100), C101(H101), C104(H104),
 C105(H105), C200(H200), C201(H201), C204(H204), C205(H205)
6.b Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;