#------------------------------------------------------------------------------
#$Date: 2016-04-05 20:59:19 +0300 (Tue, 05 Apr 2016) $
#$Revision: 181737 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/73/7037375.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7037375
loop_
_publ_author_name
'Younis, Fadi M.'
'Krieck, Sven'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Hydroamination of diphenylbutadiyne with secondary N-methyl-anilines
 using the dipotassium tetrakis(2,6-diisopropylanilino)calciate
 precatalyst.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6241
_journal_page_last               6250
_journal_paper_doi               10.1039/c5dt03818a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C30 H28 N2'
_chemical_formula_sum            'C30 H28 N2'
_chemical_formula_weight         416.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-24 deposited with the CCDC.
2015-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.94(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5309(15)
_cell_length_b                   11.255(2)
_cell_length_c                   10.6349(17)
_cell_measurement_temperature    133(2)
_cell_volume                     1152.1(3)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7660
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0428P)²+1.0579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                1700
_reflns_number_total             2507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03818a2.cif
_cod_data_source_block           FO4926
_cod_depositor_comments
'Adding full bibliography for 7037372--7037377.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7037375
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
N1 N 0.4455(2) -0.00104(19) 0.2639(2) 0.0307(5) Uani 1 1 d
C1 C 0.4573(2) -0.0504(2) 0.1469(3) 0.0290(6) Uani 1 1 d
C2 C 0.4813(3) 0.0196(3) 0.0545(3) 0.0313(6) Uani 1 1 d
H2 H 0.472(3) 0.111(3) 0.063(3) 0.052(9) Uiso 1 1 d
C3 C 0.3253(3) -0.0357(3) 0.2913(3) 0.0389(7) Uani 1 1 d
H3A H 0.303(3) -0.122(3) 0.263(3) 0.058(10) Uiso 1 1 d
H3B H 0.243(3) 0.007(3) 0.237(3) 0.041(8) Uiso 1 1 d
H3C H 0.340(3) -0.026(2) 0.389(3) 0.036(8) Uiso 1 1 d
C4 C 0.5087(3) 0.1094(2) 0.3187(2) 0.0300(6) Uani 1 1 d
C5 C 0.4412(3) 0.1949(3) 0.3631(3) 0.0379(7) Uani 1 1 d
H5 H 0.347(3) 0.179(3) 0.357(3) 0.040(8) Uiso 1 1 d
C6 C 0.5102(3) 0.2997(3) 0.4240(3) 0.0439(8) Uani 1 1 d
H6 H 0.454(3) 0.358(3) 0.454(3) 0.059(10) Uiso 1 1 d
C7 C 0.6451(3) 0.3195(3) 0.4420(3) 0.0448(8) Uani 1 1 d
H7 H 0.692(3) 0.392(3) 0.481(3) 0.057(10) Uiso 1 1 d
C8 C 0.7131(3) 0.2346(3) 0.3973(3) 0.0391(7) Uani 1 1 d
H8 H 0.809(3) 0.248(3) 0.402(3) 0.046(8) Uiso 1 1 d
C9 C 0.6459(3) 0.1312(3) 0.3362(3) 0.0346(6) Uani 1 1 d
H9 H 0.694(3) 0.075(3) 0.304(3) 0.037(8) Uiso 1 1 d
C10 C 0.4494(2) -0.1820(2) 0.1383(3) 0.0316(6) Uani 1 1 d
C11 C 0.3728(3) -0.2389(3) 0.0134(3) 0.0392(7) Uani 1 1 d
H11 H 0.317(3) -0.188(3) -0.067(3) 0.050(9) Uiso 1 1 d
C12 C 0.3704(3) -0.3618(3) 0.0049(4) 0.0485(8) Uani 1 1 d
H12 H 0.311(4) -0.404(3) -0.087(4) 0.078(12) Uiso 1 1 d
C13 C 0.4414(3) -0.4299(3) 0.1184(4) 0.0490(8) Uani 1 1 d
H13 H 0.447(4) -0.517(4) 0.120(4) 0.076(12) Uiso 1 1 d
C14 C 0.5161(3) -0.3752(3) 0.2445(4) 0.0455(8) Uani 1 1 d
H14 H 0.563(3) -0.419(3) 0.325(3) 0.041(8) Uiso 1 1 d
C15 C 0.5189(3) -0.2515(3) 0.2547(3) 0.0356(6) Uani 1 1 d
H15 H 0.569(3) -0.213(2) 0.347(3) 0.030(7) Uiso 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 N1 C4 120.8(2) . .
C1 N1 C3 117.6(2) . .
C4 N1 C3 116.9(2) . .
C2 C1 N1 121.1(2) . .
C2 C1 C10 123.8(2) . .
N1 C1 C10 115.1(2) . .
C1 C2 C2 126.6(3) . 3_655
C1 C2 H2 117.2(17) . .
C2 C2 H2 116.1(17) 3_655 .
N1 C3 H3A 108.3(18) . .
N1 C3 H3B 113.2(17) . .
H3A C3 H3B 105(3) . .
N1 C3 H3C 113.3(16) . .
H3A C3 H3C 109(2) . .
H3B C3 H3C 108(2) . .
C5 C4 C9 118.4(3) . .
C5 C4 N1 121.8(2) . .
C9 C4 N1 119.7(2) . .
C4 C5 C6 120.1(3) . .
C4 C5 H5 119.3(17) . .
C6 C5 H5 120.5(17) . .
C7 C6 C5 121.0(3) . .
C7 C6 H6 123.5(19) . .
C5 C6 H6 115.4(19) . .
C6 C7 C8 119.3(3) . .
C6 C7 H7 122(2) . .
C8 C7 H7 119(2) . .
C9 C8 C7 120.3(3) . .
C9 C8 H8 117.9(18) . .
C7 C8 H8 121.7(18) . .
C8 C9 C4 121.0(3) . .
C8 C9 H9 119.0(17) . .
C4 C9 H9 120.0(17) . .
C15 C10 C11 118.6(3) . .
C15 C10 C1 120.6(2) . .
C11 C10 C1 120.8(3) . .
C12 C11 C10 120.5(3) . .
C12 C11 H11 121.6(18) . .
C10 C11 H11 117.8(18) . .
C13 C12 C11 120.9(3) . .
C13 C12 H12 119(2) . .
C11 C12 H12 120(2) . .
C12 C13 C14 119.6(3) . .
C12 C13 H13 126(2) . .
C14 C13 H13 115(2) . .
C13 C14 C15 120.1(3) . .
C13 C14 H14 122.0(19) . .
C15 C14 H14 117.8(19) . .
C10 C15 C14 120.2(3) . .
C10 C15 H15 120.4(15) . .
C14 C15 H15 119.3(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C1 1.414(3) .
N1 C4 1.419(3) .
N1 C3 1.462(3) .
C1 C2 1.360(4) .
C1 C10 1.483(4) .
C2 C2 1.438(5) 3_655
C2 H2 1.04(3) .
C3 H3A 1.02(4) .
C3 H3B 0.95(3) .
C3 H3C 0.99(3) .
C4 C5 1.388(4) .
C4 C9 1.402(4) .
C5 C6 1.398(4) .
C5 H5 0.99(3) .
C6 C7 1.373(4) .
C6 H6 1.02(3) .
C7 C8 1.389(4) .
C7 H7 0.96(3) .
C8 C9 1.380(4) .
C8 H8 1.00(3) .
C9 H9 0.95(3) .
C10 C15 1.394(4) .
C10 C11 1.399(4) .
C11 C12 1.386(4) .
C11 H11 1.00(3) .
C12 C13 1.368(5) .
C12 H12 1.03(4) .
C13 C14 1.393(5) .
C13 H13 0.98(4) .
C14 C15 1.396(4) .
C14 H14 0.94(3) .
C15 H15 1.01(3) .
