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_7115948
_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(C22 H14 O9 Pb2), H2 O'
_chemical_formula_sum            'C44 H30 O19 Pb4'
_chemical_formula_weight         1691.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 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                 95.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.988(2)
_cell_length_b                   17.698(4)
_cell_length_c                   12.489(3)
_cell_measurement_reflns_used    6268
_cell_measurement_temperature    149.9(2)
_cell_measurement_theta_max      28.3930
_cell_measurement_theta_min      3.2550
_cell_volume                     2197.2(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 4.1 (CCDC)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      149.9(2)
_diffrn_detector_area_resol_mean 10.3795
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_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  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24817
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    15.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.303
_refine_diff_density_min         -1.807
_refine_diff_density_rms         0.288
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.379(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                4802
_reflns_number_total             5531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06587e2.cif
_cod_data_source_block           c:\monoi2
_cod_original_cell_volume        2197.1(8)
_cod_original_sg_symbol_H-M      'I 2'
_cod_database_code               7115948