The influence of anion, ligand geometry and stoichiometry on the structure and dimensionality of a series of AgI-bis(cyanobenzyl)piperazine coordination polymers
Beeching, Lianna J.; Hawes, Chris S.; Turner, David R.; Batten, Stuart R.; CrystEngComm 16 (2014) 6459–; doi:10.1039/c4ce00816b

data_7215837
_publ_section_title
;
 The influence of anion, ligand geometry and stoichiometry on the
 structure and dimensionality of a series of
 AgI-bis(cyanobenzyl)piperazine coordination polymers
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              6459
_journal_paper_doi               10.1039/c4ce00816b
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'C48 H52 Ag4 F6 N8 O8 S2, 2(C F3 O3 S), C3 H6 O'
_chemical_formula_sum            'C53 H58 Ag4 F12 N8 O15 S4'
_chemical_formula_weight         1834.79
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.623(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.839(6)
_cell_length_b                   11.480(3)
_cell_length_c                   24.597(8)
_cell_measurement_reflns_used    1851
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      21.744
_cell_measurement_theta_min      2.434
_cell_volume                     6685(3)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1157
_diffrn_reflns_av_unetI/netI     0.1146
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29608
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0996 before and 0.0665 after correction.
The Ratio of minimum to maximum transmission is 0.8247.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8054
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                4635
_reflns_number_total             8054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00816b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7215836--7215842.cif.'
_cod_database_code               7215837
_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, All C(H,H,H,H,H,H) groups, All O(H,H,H) groups
2. Restrained distances
 C52-C51_$1
 1.5 with sigma of 0.02
 C51_$1-C52_$1
 1.5 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C51-C52_$1
 1.5 with sigma of 0.02
 C52-H52A
 0.96 with sigma of 0.02
 C52-H52C
 0.96 with sigma of 0.02
 C52-H52B
 0.96 with sigma of 0.02
 H52B-H52C
 1.56 with sigma of 0.04
 H52B-H52A
 1.56 with sigma of 0.04
 H52C-H52A
 1.56 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O43(0.66667) H45D(0.66667) H45E(0.66667) H45F(0.66667)
 H45A(0.33333) H45B(0.33333) H45C(0.33333) C44(0.66667) C51(0.5) C46(0.66667)
 H46A(0.66667) H46B(0.66667) H46C(0.66667) O50(0.5) C49(0.33333) H49A(0.33333)
 H49B(0.33333) H49C(0.33333) C48(0.33333) O47(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C14(H14A,H14B), C17(H17A,H17B), C11(H11A,H11B), C13(H13A,
 H13B), C18(H18A,H18B)
5.b Me refined with riding coordinates:
 C45(H45D,H45E,H45F), C45(H45A,H45B,H45C)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C23(H23), C20(H20), C21(H21), C7(H7), C6(H6), C10(H10), C9(H9)
5.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C49(H49A,H49B,H49C)
;