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_7127530
_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_formula_moiety         'C24 H43 B1 Li1 O1 P1'
_chemical_formula_sum            'C24 H43 B Li O P'
_chemical_formula_weight         396.33
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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   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                 108.181(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.00090(4)
_cell_length_b                   9.96900(4)
_cell_length_c                   16.21840(4)
_cell_measurement_reflns_used    4898
_cell_measurement_temperature    115
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2457.89(6)
_computing_cell_refinement       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_collection       'CAD4 EXPRESS, (Straver, 1992)'
_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      115
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46009
_diffrn_reflns_theta_full        30.761
_diffrn_reflns_theta_max         30.761
_diffrn_reflns_theta_min         2.156
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4723
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.0007606
_refine_ls_shift/su_mean         0.0000284
_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: 
 0.223 0.167 0.755E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0946
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0478
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                5305
_reflns_number_total             7636
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            d0cc07072f2.cif
_cod_data_source_block           RNA220519B
_cod_depositor_comments
'Adding full bibliography for 7127530--7127534.cif.'
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C24 H43 B1 Li1 O1 P1'
_cod_database_code               7127530