Synthesis and Properties of Phenyl Phosphines with Meta-Positioned Methyl Groups and the X-ray Structure of Tris(3,5-dimethyl-4-methoxyphenyl)phosphine
Romain, Jeff K.; Ribblett, Jason W.; Byrn, Robert W.; Snyder, Richard D.; Storhoff, Bruce N.; Huffman, John C.; Organometallics 19 (2000) 2047–; doi:10.1021/om000019a

data_4077469
_publ_section_title
;
 Synthesis and Properties of Phenyl Phosphines with Meta-Positioned Methyl
 Groups and the X-ray Structure of
 Tris(3,5-dimethyl-4-methoxyphenyl)phosphine
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2047
_journal_paper_doi               10.1021/om000019a
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C27 H33 O3 P'
_chemical_formula_weight         436.531
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.320(3)
_cell_length_b                   37.838(10)
_cell_length_c                   10.216(3)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    97.
_cell_measurement_theta_max      11.34
_cell_measurement_theta_min      9.97
_cell_volume                     4762(2)
_computing_cell_refinement       'XTEL, local package'
_computing_data_collection       'NPS, local program'
_computing_data_reduction        'XTEL, local package'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    MULTAN78
_diffrn_ambient_temperature      97.
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'refurbished Picker diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.147
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4987
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         25.011
_diffrn_reflns_theta_min         3.05248
_diffrn_standards_decay_%        -0.6
_diffrn_standards_interval_count 400
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.1408
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated prism'
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.55
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.00000024(4)
_refine_ls_extinction_expression
;
    
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
    
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.4652
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         15550
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.0635
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.03F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                1823
_reflns_number_total             4189
_reflns_threshold_expression     F^2^>2.33\s(F^2^)
_cod_data_source_file            om000019a.cif
_cod_data_source_block
;
;
_cod_original_formula_sum        'C27 H33 O3 P1'
_cod_database_code               4077469