Cationic and charge-neutral calcium tetrahydroborate complexes and their use in the controlled ring-opening polymerisation of rac-lactide
Michael G. Cushion; Philip Mountford; Chem.Commun. 47 (2011) 2276–; doi:10.1039/c0cc04348f

data_7105997
_publ_section_title
;
 Cationic and charge-neutral calcium tetrahydroborate complexes and their
 use in the controlled ring-opening polymerisation of rac-lactide
;
_journal_name_full               Chem.Commun.
_journal_page_first              2276
_journal_paper_doi               10.1039/c0cc04348f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C20 H44 B1 Ca1 O5, C24 H20 B1'
_chemical_formula_sum            'C44 H64 B2 Ca O5'
_chemical_formula_weight         734.69
_chemical_name_systematic
;
[Ca(BH4)(THF)5][BPh4]
;
_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
_cell_angle_alpha                94.1835(10)
_cell_angle_beta                 103.4250(9)
_cell_angle_gamma                92.0870(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6080(2)
_cell_length_b                   14.8383(3)
_cell_length_c                   15.2496(3)
_cell_measurement_reflns_used    8531
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2105.85(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15200
_diffrn_reflns_theta_full        26.377
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         5.114
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.16
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6134
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.004605
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.70 1.39 1.34 0.250 0.256
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1119
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0815
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6818
_reflns_number_total             9500
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.00
_oxford_diffrn_Wilson_scale      2.76
_oxford_refine_ls_r_factor_ref   0.0723
_oxford_refine_ls_scale          0.6241(15)
_oxford_reflns_number_all        9500
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            C0CC04348F.TXT
_cod_data_source_block           COMPOUND_1-BPh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C44 H64 B2 Ca1 O5'
_cod_database_code               7105997