Synthesis and Characterization of Multi-Alkali-Metal Tetraphenolates and Application in Ring-Opening Polymerization of Lactide
Jinjin Zhang; Chunli Jian; Yuan Gao; Lei Wang; Ning Tang; Jincai Wu; Inorganic Chemistry 51 (2012) 13380–13389; doi:10.1021/ic302193y

data_4331365
_publ_section_title
;
 Synthesis and Characterization of Multi-Alkali-Metal Tetraphenolates and
 Application in Ring-Opening Polymerization of Lactide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13380
_journal_page_last               13389
_journal_paper_doi               10.1021/ic302193y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C88 H132 K3 O10'
_chemical_formula_weight         1467.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 106.594(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.298(9)
_cell_length_b                   14.342(4)
_cell_length_c                   19.574(5)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.03
_cell_measurement_theta_min      2.30
_cell_volume                     9497(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1553
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23971
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.9607
_exptl_absorpt_correction_T_min  0.9357
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_description       block
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         14265
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.2214
_refine_ls_R_factor_gt           0.0826
_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^)+(0.1193P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.2548
_reflns_number_gt                5414
_reflns_number_total             14265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302193y_si_001_7.cif
_cod_data_source_block           m-3k
_cod_database_code               4331365