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_7105998
_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         'C48 H62 B2 Ca1 N6 O2, 2 (C4 H8 O)'
_chemical_formula_sum            'C56 H78 B2 Ca N6 O4'
_chemical_formula_weight         960.98
_chemical_name_systematic
;
[Ca{HC(Me2pz)3}(BH4)(THF)2][BPh4] . 2(THF)
;
_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                82.3488(12)
_cell_angle_beta                 82.0004(12)
_cell_angle_gamma                80.4508(7)
_cell_formula_units_Z            2
_cell_length_a                   10.3958(2)
_cell_length_b                   15.0936(4)
_cell_length_c                   17.5126(4)
_cell_measurement_reflns_used    8526
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     2666.36(11)
_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 0.984
_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  0.019
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15844
_diffrn_reflns_theta_full        25.032
_diffrn_reflns_theta_max         25.032
_diffrn_reflns_theta_min         5.172
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         7488
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.019404
_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:
0.409 0.325 0.243 0.983E-01 0.606E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0594
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0464
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                7647
_reflns_number_total             9271
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.35
_oxford_diffrn_Wilson_scale      0.62
_oxford_refine_ls_r_factor_ref   0.0440
_oxford_refine_ls_scale          0.3114(4)
_oxford_reflns_number_all        9271
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            C0CC04348F.TXT
_cod_data_source_block           COMPOUND_2-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        'C56 H78 B2 Ca1 N6 O4'
_cod_database_code               7105998