Calcium-Mediated Catalytic Synthesis of 1-(Diorganylamino)-1,4-diphenyl-4-(diphenylphosphanyl)buta-1,3-dienes.
Younis, Fadi M.; Krieck, Sven; Al-Shboul, Tareq M A; Görls, Helmar; Westerhausen, Matthias; Inorganic chemistry 55 (2016) 4676–4682; doi:10.1021/acs.inorgchem.6b00586

data_4347774
_publ_section_title
;
 Calcium-Mediated Catalytic Synthesis of
 1-(Diorganylamino)-1,4-diphenyl-4-(diphenylphosphanyl)buta-1,3-dienes.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4676
_journal_page_last               4682
_journal_paper_doi               10.1021/acs.inorgchem.6b00586
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H32 N P'
_chemical_formula_sum            'C36 H32 N P'
_chemical_formula_weight         509.60
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 101.550(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0756(2)
_cell_length_b                   18.8919(5)
_cell_length_c                   12.6638(4)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.71
_cell_volume                     1424.11(8)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9749
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.032
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6311
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.9132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                5117
_reflns_number_total             6311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00586_si_002.cif
_cod_data_source_block           FO5738
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347774