Cyclic versus Polymeric Supramolecular Architectures in Metal Complexes of Dinucleating Ligands: Silver(I) Trifluoromethanesulfonate Complexes of the Isomers of Bis(di(1H-pyrazolyl)methyl)-1,1′-biphenyl.
Gardinier, James R.; Tatlock, Heidi M.; Hewage, Jeewantha S.; Lindeman, Sergey V.; Crystal Growth & Design 13 (2013) 3864–; doi:10.1021/cg400466k

data_4508127
_publ_section_title
;
 Cyclic versus Polymeric Supramolecular Architectures in Metal Complexes
 of Dinucleating Ligands: Silver(I) Trifluoromethanesulfonate Complexes of
 the Isomers of Bis(di(1H-pyrazolyl)methyl)-1,1&#x2032;-biphenyl.
;
_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3864
_journal_paper_doi               10.1021/cg400466k
_journal_volume                  13
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C52 H44 Ag2 N16, 2(C F3 O3 S), 0.5(C4 H10 O), 2(C2 H3 N)'
_chemical_formula_sum            'C60 H55 Ag2 F6 N18 O6.5 S2'
_chemical_formula_weight         1526.08
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-08-30
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.34228(16)
_cell_length_b                   14.34228(16)
_cell_length_c                   32.9099(6)
_cell_measurement_reflns_used    13528
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8077
_cell_measurement_theta_min      3.3586
_cell_volume                     6769.60(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -30.00   -5.00   1.0000    1.9600
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   37.0000 -180.0000 25

  2 omega  -69.00   33.00   1.0000    1.9600
omega____ theta____ kappa____ phi______ frames
    -      -40.6487   57.0000   30.0000 102

  3 omega  124.00  177.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000   90.0000 53

  4 omega   33.00   73.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000   60.0000 40

  5 omega   29.00   55.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -30.0000 -180.0000 26

  6 omega   97.00  148.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000  150.0000 51

  7 omega   37.00   98.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000 -150.0000 61

  8 omega -119.00   -7.00   1.0000    1.9600
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -77.0000   30.0000 112

  9 omega -117.00  -14.00   1.0000    1.9600
omega____ theta____ kappa____ phi______ frames
    -      -40.6487  -37.0000 -120.0000 103

 10 omega   32.00   98.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  -45.0000  120.0000 66

 11 omega   77.00  178.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378   30.0000  120.0000 101

 12 omega   94.00  178.00   1.0000    7.8400
omega____ theta____ kappa____ phi______ frames
    -      107.0378  125.0000 -150.0000 84
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0822996000
_diffrn_orient_matrix_UB_12      0.0058009000
_diffrn_orient_matrix_UB_13      -0.0299403000
_diffrn_orient_matrix_UB_21      0.0661987000
_diffrn_orient_matrix_UB_22      0.0225007000
_diffrn_orient_matrix_UB_23      0.0354508000
_diffrn_orient_matrix_UB_31      0.0187823000
_diffrn_orient_matrix_UB_32      -0.1050630000
_diffrn_orient_matrix_UB_33      0.0060087000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            32806
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.97
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.900
_exptl_absorpt_correction_T_max  0.381
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3092
_exptl_crystal_size_max          0.5483
_exptl_crystal_size_mid          0.3935
_exptl_crystal_size_min          0.2661
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_extinction_coef       0.00059(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   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0794P)^2^+8.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                6323
_reflns_number_total             6769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400466k_si_001.cif
_cod_data_source_block           Ag(L34)OTf_5
_cod_original_cell_volume        6769.60(17)
_cod_original_formula_sum        'C60 H55 Ag2 F6 N18 O6.50 S2'
_cod_database_code               4508127
_chemical_oxdiff_formula         'C54 H44 O6 N16 F6 S2 Ag2'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97