Synthesis and rac-lactide ring-opening polymerisation studies of new alkaline earth tetrahydroborate complexes.
Collins, Richard A.; Unruangsri, Junjuda; Mountford, Philip; Dalton transactions (Cambridge, England : 2003) 42 (2013) 759–769; doi:10.1039/c2dt32151c

data_7020849
_publ_section_title
;
 Synthesis and rac-lactide ring-opening polymerisation studies of new
 alkaline earth tetrahydroborate complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              759
_journal_page_last               769
_journal_paper_doi               10.1039/c2dt32151c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C37 H61 B1 Ca1 N2 O2'
_chemical_formula_sum            'C37 H61 B Ca N2 O2'
_chemical_formula_weight         616.79
_chemical_name_systematic
;
Ca{HC(C(Me)NAr')2}(BH4)(THF)2
;
_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   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.6264(6)
_cell_angle_beta                 81.3505(6)
_cell_angle_gamma                70.8144(7)
_cell_formula_units_Z            4
_cell_length_a                   14.6535(2)
_cell_length_b                   15.6432(2)
_cell_length_c                   17.6883(3)
_cell_measurement_reflns_used    16188
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3699.07(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30444
_diffrn_reflns_theta_full        25.286
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         5.096
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.25
_refine_ls_extinction_coef       200(90)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1353
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         9749
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.0009231
_refine_ls_shift/su_mean         0.0000214
_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:
1.38 1.53 1.51 0.596 0.382
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0674
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0407
_reflns_limit_h_max              19
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                10934
_reflns_number_total             16772
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      10.24
_oxford_refine_ls_r_factor_ref   0.0424
_oxford_refine_ls_scale          0.3215(4)
_oxford_reflns_number_all        16772
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c2dt32151c.txt
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C37 H61 B1 Ca1 N2 O2'
_cod_database_code               7020849