Interplay between lead carboxylate and Ti or Zr isopropoxides in solution routes to perovskites: synthesis, molecular structures and reactivity of single source non-oxo Pb-Zr and Pb-Ti carboxylatoalkoxides supported by 2-ethylhexanoate ligands.
Brethon, Anne; Hubert-Pfalzgraf, Liliane G; Daran, Jean-Claude; Dalton transactions (Cambridge, England : 2003)  (2006) 250–257; doi:10.1039/b513142c

data_7006696
_publ_section_title
;
 Interplay between lead carboxylate and Ti or Zr isopropoxides in
 solution routes to perovskites: synthesis, molecular structures and
 reactivity of single source non-oxo Pb-Zr and Pb-Ti
 carboxylatoalkoxides supported by 2-ethylhexanoate ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              250
_journal_page_last               257
_journal_paper_doi               10.1039/b513142c
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C54 H112 O17 Pb2 Zr2'
_chemical_formula_sum            'C54 H112 O17 Pb2 Zr2'
_chemical_formula_weight         1630.26
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                85.559(8)
_cell_angle_beta                 83.667(7)
_cell_angle_gamma                76.410(8)
_cell_formula_units_Z            2
_cell_length_a                   11.3776(10)
_cell_length_b                   13.1183(12)
_cell_length_c                   26.190(3)
_cell_measurement_reflns_used    6226
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      3.31
_cell_volume                     3771.0(7)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
1 omega -54.00 60.75 0.7500 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 26.0000 -79.0000 0.0000 0.0000 0.0000 153

2 omega -54.00 60.75 0.7500 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 26.0000 -79.0000 90.0000 0.0000 0.0000 153

3 omega -54.00 60.75 0.7500 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 26.0000 -79.0000 180.0000 0.0000 0.0000 153

4 omega -54.00 60.75 0.7500 20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 26.0000 -79.0000 270.0000 0.0000 0.0000 153

;
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      0.0588890499
_diffrn_orient_matrix_UB_12      -0.0325913467
_diffrn_orient_matrix_UB_13      -0.0049040321
_diffrn_orient_matrix_UB_21      0.0217084697
_diffrn_orient_matrix_UB_22      0.0257243571
_diffrn_orient_matrix_UB_23      0.0185913572
_diffrn_orient_matrix_UB_31      -0.0145593022
_diffrn_orient_matrix_UB_32      -0.0371382891
_diffrn_orient_matrix_UB_33      0.0193635544
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20240
_diffrn_reflns_theta_full        23.21
_diffrn_reflns_theta_max         23.21
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.772
_exptl_absorpt_correction_T_max  0.48701
_exptl_absorpt_correction_T_min  0.30423
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat box'
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.868
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         10765
_refine_ls_number_restraints     772
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.110
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0809P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                6832
_reflns_number_total             10765
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b513142c.txt
_cod_data_source_block           AB43
_cod_original_cell_volume        3771.0(6)
_cod_database_code               7006696