A facile single crystal to single crystal transition with significant structural contraction on desolvation
Jane V. Knichal; William J. Gee; Andrew D. Burrows; Paul R. Raithby; Simon J. Teat; Chick C. Wilson; Chem.Commun. 50 (2014) 14436–; doi:10.1039/C4cc06587E

data_7115949
_publ_section_title
;
 A facile single crystal to single crystal transition with significant
 structural contraction on desolvation
;
_journal_name_full               Chem.Commun.
_journal_page_first              14436
_journal_paper_doi               10.1039/C4cc06587E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '2(C11 H8 O5 Pb), H2 O'
_chemical_formula_sum            'C22 H18 O11 Pb2'
_chemical_formula_weight         872.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.037(2)
_cell_length_b                   17.698(4)
_cell_length_c                   12.687(3)
_cell_measurement_reflns_used    2209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3283
_cell_measurement_theta_min      3.2273
_cell_volume                     2238.0(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'POV-Ray, version 3.6, 2004'
_computing_publication_material  'ENCIFER 1.4 (CCDC)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details
;
  1 omega  -91.00  -19.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0553  160.0000  115.0000 72

  2 omega  -13.00   76.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2272   57.0000   90.0000 89

  3 omega  -60.00   15.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2272  -57.0000  -60.0000 75

;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185890000
_diffrn_orient_matrix_UB_12      0.0075288000
_diffrn_orient_matrix_UB_13      0.0811908000
_diffrn_orient_matrix_UB_21      0.0046415000
_diffrn_orient_matrix_UB_22      0.0388994000
_diffrn_orient_matrix_UB_23      -0.0120683000
_diffrn_orient_matrix_UB_31      -0.0529415000
_diffrn_orient_matrix_UB_32      0.0060518000
_diffrn_orient_matrix_UB_33      -0.0235516000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6767
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    15.088
_exptl_absorpt_correction_T_max  0.1523
_exptl_absorpt_correction_T_min  0.0649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.866
_refine_diff_density_min         -2.270
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2606
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                2043
_reflns_number_total             2606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06587e2.cif
_cod_data_source_block           c:\monoi2a
_cod_original_cell_volume        2238.1(8)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7115949