Synthesis and reactivity of phosphine borohydride compounds.
Ayyappan, Ramaraj; Coppel, Yannick; Vendier, Laure; Ghosh, Sundargopal; Sabo-Etienne, Sylviane; Bontemps, Sébastien; Chemical communications (Cambridge, England) 57 (2021) 375–378; doi:10.1039/d0cc07072f

data_7127534
_publ_section_title
;
 Synthesis and reactivity of phosphine borohydride compounds.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              375
_journal_page_last               378
_journal_paper_doi               10.1039/d0cc07072f
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C80 H138 B2 Li2 O4 P2'
_chemical_formula_sum            'C80 H138 B2 Li2 O4 P2'
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
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_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2020-10-19 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.092900(14)
_cell_length_b                   19.47580(2)
_cell_length_c                   35.92390(3)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    110
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     7761.111(14)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            89157
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_diffrn_reflns_theta_min         1.134
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_exptl_absorpt_coefficient_mu    0.102
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_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
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_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 6073 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8344
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         14030
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.0011672
_refine_ls_shift/su_mean         0.0000554
_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: 
 0.451 0.379 0.271 0.308E-01 
;
_refine_ls_weighting_scheme      calc
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_reflns_limit_k_max              25
_reflns_limit_k_min              0
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_reflns_number_total             17924
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            d0cc07072f2.cif
_cod_data_source_block           Ramaraj190620
_cod_depositor_comments
'Adding full bibliography for 7127530--7127534.cif.'
_cod_original_cell_volume        7761.110(15)
_cod_original_sg_symbol_Hall     'P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               7127534
_oxford_hooft_y                  -0.01(3)
_oxford_bijvoet_difference       0.01(3)