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_1542773
_publ_section_title
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 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         'C40 H16 Ag4 F28 N4 O8, 3(C7 H8)'
_chemical_formula_sum            'C61 H40 Ag4 F28 N4 O8'
_chemical_formula_weight         1920.45
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-04-10 # Formatted by IUCr publCIF system
;
_cell_angle_alpha                72.401(3)
_cell_angle_beta                 86.598(3)
_cell_angle_gamma                82.882(3)
_cell_formula_units_Z            1
_cell_length_a                   10.6531(7)
_cell_length_b                   11.2628(7)
_cell_length_c                   14.4311(10)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.116
_cell_measurement_theta_min      2.403
_cell_volume                     1637.30(19)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.969
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25299
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.557
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0967 before and 0.0640 after correction.
The Ratio of minimum to maximum transmission is 0.8435.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       plate
_exptl_crystal_F_000             938
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.325
_refine_diff_density_min         -1.726
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.0027(6)
_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   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0650P)^2^+14.5417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6165
_reflns_number_total             7283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bi5040.cif
_cod_data_source_block           1-tol.tol
_cod_database_code               1542773
_publcif_datablock.id            {dadff06d-799b-40e8-b246-164ea9928ead}
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.614
_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. Others
 Sof(C2')=Sof(F2Y)=Sof(F2Z)=Sof(C3')=Sof(F3Z)=Sof(F3Y)=Sof(C4')=Sof(F4Z)=
 Sof(F4Y)=Sof(F4X)=1-FVAR(1)
 Sof(C2)=Sof(F2A)=Sof(F2B)=Sof(C3)=Sof(F3B)=Sof(F3A)=Sof(C4)=Sof(F4A)=Sof(F4B)=
 Sof(F4C)=FVAR(1)
 Fixed Sof: H52(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) H60(0.5) C63(0.5)
 H63A(0.5) H63B(0.5) H63C(0.5) H71(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C105(H105), C104(H104), C101(H101), C100(H100), C204(H204), C205(H205),
 C200(H200), C201(H201), C51(H51), C50(H50), C52(H52), C60(H60), C61(H61),
 C62(H62), C70(H70), C71(H71), C73(H73)
3.b Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C63(H63A,H63B,H63C), C72(H72A,H72B,H72C)
;
_olex2_submission_special_instructions 'No special instructions were received'