Synthetic and Structural Investigations of Monomeric Dilithium Boraamidinates and Bidentate NBNCN Ligands with Bulky N-Bonded Groups
T. Chivers; C. Fedorchuk; M. Parvez; Inorganic Chemistry 43 (2004) 2643–2653; doi:10.1021/ic0352755

data_4310845
_publ_section_title
;
 Synthetic and Structural Investigations of Monomeric Dilithium
 Boraamidinates and Bidentate NBNCN Ligands with Bulky N-Bonded Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2643
_journal_page_last               2653
_journal_paper_doi               10.1021/ic0352755
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C30 H51 B Li2 N2 O2'
_chemical_formula_weight         496.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 117.523(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.019(3)
_cell_length_b                   18.461(3)
_cell_length_c                   20.330(4)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.20
_cell_volume                     6330(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics
'Cameron (WinGX v1.64-04), Ortep (SHELXTL-NT v5.1, Bruker)'
_computing_publication_material  'WinGX v1.64-05 (L.J. Farrugia)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Kappa CCD (Nonius, FR540C)'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0707
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19425
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.9852
_exptl_absorpt_correction_type   'multi-scan method'
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         11128
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+3.3300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                7142
_reflns_number_total             11128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0352755si20040218_033734_5.cif
_cod_data_source_block           7b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6330.2(19)
_cod_database_code               4310845