Tri(1-adamantyl)phosphine: Expanding the Boundary of Electron-Releasing Character Available to Organophosphorus Compounds.
Chen, Liye; Ren, Peng; Carrow, Brad P.; Journal of the American Chemical Society 138 (2016) 6392–6395; doi:10.1021/jacs.6b03215

data_4130419
_publ_section_title
;
 Tri(1-adamantyl)phosphine: Expanding the Boundary of Electron-Releasing
 Character Available to Organophosphorus Compounds.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6392
_journal_page_last               6395
_journal_paper_doi               10.1021/jacs.6b03215
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C38 H53 N O P Pd, C7 H7 O3 S, C4 H8 O'
_chemical_formula_sum            'C49 H68 N O5 P Pd S'
_chemical_formula_weight         920.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_Int_Tables_number      7
_audit_creation_date             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.448(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7563(8)
_cell_length_b                   11.5192(8)
_cell_length_c                   17.1433(12)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      3.79
_cell_volume                     2123.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9952
_diffrn_measured_fraction_theta_max 0.9952
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57768
_diffrn_reflns_theta_full        33.2314
_diffrn_reflns_theta_max         33.23
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0514 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.9369.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.4396
_exptl_crystal_description       shard
_exptl_crystal_F_000             970.8507
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.5706
_refine_diff_density_min         -0.3638
_refine_diff_density_rms         0.0713
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_d_res_high            0.6485
_refine_ls_d_res_low             11.5192
_refine_ls_goodness_of_fit_ref   1.0309
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    110
_refine_ls_number_parameters     524
_refine_ls_number_reflns         14247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0309
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.746
_reflns_limit_h_max              14
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              26
_reflns_limit_l_min              -26
_reflns_number_gt                13585
_reflns_number_total             14247
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja6b03215_si_003.cif
_cod_data_source_block           mo_lc10_0m
_cod_original_sg_symbol_Hall     ' P -2yc (x-z,y,z)'
_cod_database_code               4130419
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C33(H33), C23(H23), C18(H18), C11(H11), C21(H21), C13(H13),
 C38(H38), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C22(H22a,H22b), C32(H32a,H32b), C36(H36a,H36b), C14(H14a,
 H14b), C20(H20a,H20b), C27(H27a,H27b), C30(H30a,H30b), C16(H16a,H16b),
 C24(H24a,H24b), C10(H10a,H10b), C12(H12a,H12b), C17(H17a,H17b), C26(H26a,H26b),
  C34(H34a,H34b), C47(H47a,H47b), C25(H25a,H25b), C48(H48a,H48b), C37(H37a,
 H37b), C46(H46a,H46b), C35(H35a,H35b), C49(H49a,H49b)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C4(H4), C44(H44), C45(H45), C41(H41), C42(H42),
 N008(H008)
2.d Idealised Me refined as rotating group:
 C39(H39a,H39b,H39c), C1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'