Formation of the monoanion [Ar*P(BH3)(µ-BH2)2H]‒ with a symmetrically bridging hydride from the attempted synthesis of the dianion [Ar*P(BH3)3]2‒
Rudzevich, Valentyn L.; Gornitzka, Heinz; Romanenko, Vadim D.; Bertrand, Guy; Chemical Communications  (2001) 1634–; doi:10.1039/b105030n

data_7115042
_publ_section_title
;
 Formation of the monoanion [Ar*P(BH3)(&#x00B5;-BH2)2H]-- with a
 symmetrically bridging hydride from the attempted synthesis of the
 dianion [Ar*P(BH3)3]2--
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1634
_journal_paper_doi               10.1039/b105030n
_journal_year                    2001
_chemical_formula_sum            'C30 H60 B2 Li O3 P'
_chemical_formula_weight         528.31
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4853(5)
_cell_length_b                   11.0044(5)
_cell_length_c                   32.8968(16)
_cell_measurement_reflns_used    7935
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.236
_cell_measurement_theta_min      2.226
_cell_volume                     3433.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            18214
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.811550
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7012
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.5772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                5840
_reflns_number_total             7012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105030n.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7115042