#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/24/4072413.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_4072413
loop_
_publ_author_name
'Tan, Runyu'
'Jia, Peng'
'Rao, Yingli'
'Jia, Wenli'
'Hadzovic, Alen'
'Yu, Qing'
'Li, Xia'
'Song, Datong'
_publ_section_title
;
 Diplatinum Complexes Supported by Novel Tetradentate Ligands with
 Quinoline Functionalities for Tandem C−Cl Activation and
 Dearomatization
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6614
_journal_paper_doi               10.1021/om800893r
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C13 H14 Br N'
_chemical_formula_weight         264.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.5474(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7872(2)
_cell_length_b                   9.4647(3)
_cell_length_c                   12.7521(3)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.75
_cell_volume                     1219.13(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    3.339
_exptl_absorpt_correction_T_max  0.380
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0381
_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)+(0.0386P)²+3.1482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                1873
_reflns_number_total             2135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800893r_si_001.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4072413
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_refinement_flags
Br1 Br 0.17053(3) 0.12229(4) 0.00182(3) 0.02819(15) Uani 1 1 d .
N1 N 0.3733(3) 0.3073(3) 0.1758(3) 0.0308(7) Uani 1 1 d .
C1 C 0.4580(4) 0.3969(5) 0.2424(4) 0.0411(10) Uani 1 1 d .
H1A H 0.4955 0.4664 0.2088 0.049 Uiso 1 1 calc R
C2 C 0.4968(4) 0.3971(5) 0.3594(4) 0.0394(10) Uani 1 1 d .
H2A H 0.5572 0.4660 0.4026 0.047 Uiso 1 1 calc R
C3 C 0.4467(4) 0.2971(4) 0.4101(3) 0.0293(8) Uani 1 1 d .
H3A H 0.4718 0.2953 0.4893 0.035 Uiso 1 1 calc R
C4 C 0.3569(3) 0.1960(4) 0.3436(3) 0.0228(7) Uani 1 1 d .
C5 C 0.3021(3) 0.0883(4) 0.3910(3) 0.0240(7) Uani 1 1 d .
H5A H 0.3266 0.0830 0.4701 0.029 Uiso 1 1 calc R
C6 C 0.2148(3) -0.0080(4) 0.3255(3) 0.0249(7) Uani 1 1 d .
C7 C 0.1777(3) 0.0042(4) 0.2073(3) 0.0229(7) Uani 1 1 d .
H7A H 0.1165 -0.0612 0.1602 0.027 Uiso 1 1 calc R
C8 C 0.2286(3) 0.1082(4) 0.1605(3) 0.0207(7) Uani 1 1 d .
C9 C 0.3217(3) 0.2073(4) 0.2257(3) 0.0213(7) Uani 1 1 d .
C10 C 0.1514(4) -0.1254(4) 0.3725(3) 0.0389(10) Uani 1 1 d .
C11 C 0.0016(6) -0.0989(6) 0.3337(4) 0.0622(9) Uani 1 1 d .
H11A H -0.0353 -0.0968 0.2517 0.093 Uiso 1 1 calc R
H11B H -0.0151 -0.0082 0.3634 0.093 Uiso 1 1 calc R
H11C H -0.0406 -0.1749 0.3613 0.093 Uiso 1 1 calc R
C12 C 0.1788(6) -0.2675(6) 0.3300(4) 0.0622(9) Uani 1 1 d .
H12A H 0.2746 -0.2836 0.3556 0.093 Uiso 1 1 calc R
H12B H 0.1426 -0.2682 0.2479 0.093 Uiso 1 1 calc R
H12C H 0.1369 -0.3424 0.3589 0.093 Uiso 1 1 calc R
C13 C 0.2059(6) -0.1290(6) 0.5003(4) 0.0622(9) Uani 1 1 d .
H13A H 0.3015 -0.1467 0.5265 0.093 Uiso 1 1 calc R
H13B H 0.1622 -0.2046 0.5268 0.093 Uiso 1 1 calc R
H13C H 0.1890 -0.0381 0.5295 0.093 Uiso 1 1 calc R
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'
Br Br -0.2901 2.4595 '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
C1 N1 C9 116.8(3)
N1 C1 C2 124.7(4)
C3 C2 C1 119.0(4)
C2 C3 C4 119.2(3)
C3 C4 C5 122.1(3)
C3 C4 C9 117.2(3)
C5 C4 C9 120.7(3)
C6 C5 C4 121.4(3)
C5 C6 C7 118.1(3)
C5 C6 C10 123.5(3)
C7 C6 C10 118.4(3)
C8 C7 C6 121.1(3)
C7 C8 C9 122.3(3)
C7 C8 Br1 119.0(3)
C9 C8 Br1 118.7(2)
N1 C9 C8 120.6(3)
N1 C9 C4 123.0(3)
C8 C9 C4 116.4(3)
C12 C10 C13 108.1(4)
C12 C10 C6 109.5(4)
C13 C10 C6 112.1(3)
C12 C10 C11 110.2(4)
C13 C10 C11 108.3(4)
C6 C10 C11 108.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Br1 C8 1.902(3)
N1 C1 1.315(5)
N1 C9 1.364(5)
C1 C2 1.400(6)
C2 C3 1.361(6)
C3 C4 1.413(5)
C4 C5 1.415(5)
C4 C9 1.419(5)
C5 C6 1.365(5)
C6 C7 1.422(5)
C6 C10 1.533(5)
C7 C8 1.361(5)
C8 C9 1.412(5)
C10 C12 1.517(7)
C10 C13 1.527(6)
C10 C11 1.536(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 19029601
