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_7115947
_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         'C20 H8 O8 Pb2'
_chemical_formula_sum            'C20 H8 O8 Pb2'
_chemical_formula_weight         790.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.148(3)
_cell_angle_beta                 91.407(3)
_cell_angle_gamma                107.941(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3790(4)
_cell_length_b                   10.0130(3)
_cell_length_c                   10.3180(4)
_cell_measurement_reflns_used    5621
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      2.92
_cell_volume                     904.22(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_sigmaI/netI    0.1217
_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       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13225
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.58
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    18.645
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.4877
_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    2.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.821
_refine_diff_density_min         -2.454
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                3486
_reflns_number_total             5621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06587e2.cif
_cod_data_source_block           c:\bath1724
_cod_database_code               7115947