#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:36:11 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180087 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/33/7053375.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_7053375
loop_
_publ_author_name
'Franc, Grégory'
'Badetti, Elena'
'Duhayon, Carine'
'Coppel, Yannick'
'Turrin, Cédric-Olivier'
'Majoral, Jean-Pierre'
'Sebastián, Rosa-María'
'Caminade, Anne-Marie'
_publ_section_title
;
 An efficient synthesis combining phosphorus dendrimers and 15-membered
 triolefinic azamacrocycles: towards the stabilization of platinum
 nanoparticles
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              547
_journal_paper_doi               10.1039/b9nj00568d
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C42 H64 Br2 N2 O4 S2'
_chemical_formula_sum            'C42 H64 Br2 N2 O4 S2'
_chemical_formula_weight         884.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-03-30
_audit_creation_method           CRYSTALS_ver_12.51
_cell_angle_alpha                101.754(5)
_cell_angle_beta                 96.690(5)
_cell_angle_gamma                93.917(5)
_cell_formula_units_Z            1
_cell_length_a                   6.265(5)
_cell_length_b                   12.133(5)
_cell_length_c                   15.070(5)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    180
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     1108.9(11)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10430
_diffrn_reflns_theta_full        27.023
_diffrn_reflns_theta_max         29.057
_diffrn_reflns_theta_min         2.946
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.962
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3711
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.000616
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
3.99 -1.39 2.94
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0425
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0377
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                3711
_reflns_number_total             5890
_reflns_threshold_expression     I>3.0σ(I)
_cod_data_source_file            b9nj00568d.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7053375
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
C1 C 0.9550(5) 0.3263(2) 0.74912(17) 0.0439 1.0000 Uani .
C2 C 0.8232(4) 0.2379(2) 0.67744(15) 0.0325 1.0000 Uani .
C3 C 0.7389(3) 0.25710(18) 0.59826(14) 0.0279 1.0000 Uani .
C4 C 0.6045(3) 0.16946(18) 0.52466(13) 0.0248 1.0000 Uani .
C5 C 0.9202(3) 0.12252(17) 0.44074(13) 0.0228 1.0000 Uani .
C6 C 0.9376(3) 0.00815(18) 0.46363(13) 0.0236 1.0000 Uani .
C7 C 0.6653(3) 0.18774(16) 0.26588(13) 0.0191 1.0000 Uani .
C8 C 0.6455(3) 0.30548(16) 0.27831(13) 0.0211 1.0000 Uani .
C9 C 0.7165(3) 0.36057(17) 0.21315(13) 0.0247 1.0000 Uani .
C10 C 0.8072(3) 0.30644(17) 0.13909(13) 0.0253 1.0000 Uani .
C11 C 0.8332(3) 0.19219(17) 0.13076(13) 0.0254 1.0000 Uani .
C12 C 0.7671(3) 0.13023(16) 0.19341(13) 0.0206 1.0000 Uani .
C13 C 0.8125(3) 0.00629(16) 0.17606(14) 0.0240 1.0000 Uani .
C14 C 1.0369(4) -0.0115(2) 0.14938(16) 0.0328 1.0000 Uani .
C15 C 0.6403(4) -0.06434(19) 0.10225(17) 0.0356 1.0000 Uani .
C16 C 0.8758(4) 0.37092(18) 0.06887(15) 0.0307 1.0000 Uani .
C17 C 1.0910(5) 0.3431(3) 0.0394(2) 0.0542 1.0000 Uani .
C18 C 0.7020(5) 0.3513(3) -0.01301(19) 0.0535 1.0000 Uani .
C19 C 0.5524(3) 0.37824(17) 0.35688(14) 0.0257 1.0000 Uani .
C20 C 0.3350(4) 0.4148(2) 0.32196(18) 0.0439 1.0000 Uani .
C21 C 0.7109(5) 0.4807(2) 0.40485(17) 0.0463 1.0000 Uani .
Br1 Br 1.25752(5) 0.29349(3) 0.75976(2) 0.0581 1.0000 Uani .
N1 N 0.7009(2) 0.16086(14) 0.43891(11) 0.0207 1.0000 Uani .
O1 O 0.3365(2) 0.15848(13) 0.35520(10) 0.0272 1.0000 Uani .
O2 O 0.5368(2) -0.00437(12) 0.31062(10) 0.0284 1.0000 Uani .
S1 S 0.54119(7) 0.11553(4) 0.34194(3) 0.0199 1.0000 Uani .
H21 H 0.7984 0.1604 0.6896 0.0392 1.0000 Uiso R
H31 H 0.7662 0.3347 0.5866 0.0337 1.0000 Uiso R
H41 H 0.6008 0.0947 0.5430 0.0308 1.0000 Uiso R
H42 H 0.4542 0.1919 0.5153 0.0308 1.0000 Uiso R
H51 H 1.0200 0.1791 0.4875 0.0290 1.0000 Uiso R
H52 H 0.9662 0.1194 0.3790 0.0290 1.0000 Uiso R
H61 H 0.8509 -0.0588 0.4221 0.0294 1.0000 Uiso R
H91 H 0.7010 0.4433 0.2204 0.0302 1.0000 Uiso R
H111 H 0.9021 0.1526 0.0781 0.0318 1.0000 Uiso R
H131 H 0.8028 -0.0209 0.2339 0.0293 1.0000 Uiso R
H141 H 1.0580 -0.0939 0.1388 0.0393 1.0000 Uiso R
H142 H 1.1483 0.0314 0.1997 0.0393 1.0000 Uiso R
H143 H 1.0515 0.0163 0.0921 0.0393 1.0000 Uiso R
H151 H 0.6712 -0.1454 0.0912 0.0408 1.0000 Uiso R
H152 H 0.6422 -0.0364 0.0443 0.0408 1.0000 Uiso R
H153 H 0.4950 -0.0573 0.1230 0.0408 1.0000 Uiso R
H161 H 0.8894 0.4533 0.0979 0.0374 1.0000 Uiso R
H171 H 1.1267 0.3880 -0.0066 0.0700 1.0000 Uiso R
H172 H 1.2051 0.3622 0.0937 0.0700 1.0000 Uiso R
H173 H 1.0840 0.2606 0.0114 0.0700 1.0000 Uiso R
H181 H 0.7485 0.3939 -0.0588 0.0671 1.0000 Uiso R
H182 H 0.5648 0.3783 0.0073 0.0671 1.0000 Uiso R
H183 H 0.6781 0.2687 -0.0415 0.0671 1.0000 Uiso R
H191 H 0.5272 0.3310 0.4025 0.0317 1.0000 Uiso R
H201 H 0.2753 0.4624 0.3739 0.0552 1.0000 Uiso R
H202 H 0.3551 0.4595 0.2742 0.0552 1.0000 Uiso R
H203 H 0.2323 0.3462 0.2949 0.0552 1.0000 Uiso R
H211 H 0.6458 0.5268 0.4559 0.0536 1.0000 Uiso R
H212 H 0.8482 0.4540 0.4300 0.0536 1.0000 Uiso R
H213 H 0.7421 0.5281 0.3600 0.0536 1.0000 Uiso R
H11 H 0.8998 0.3283 0.8090 0.0512 1.0000 Uiso R
H12 H 0.9440 0.4014 0.7321 0.0512 1.0000 Uiso R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 Br1 . 109.97(19) yes
C2 . C1 H11 . 109.4 no
Br1 . C1 H11 . 109.5 no
C2 . C1 H12 . 109.2 no
Br1 . C1 H12 . 109.3 no
H11 . C1 H12 . 109.5 no
C1 . C2 C3 . 122.8(2) yes
C1 . C2 H21 . 118.4 no
C3 . C2 H21 . 118.8 no
C2 . C3 C4 . 123.9(2) yes
C2 . C3 H31 . 118.1 no
C4 . C3 H31 . 118.0 no
C3 . C4 N1 . 108.99(16) yes
C3 . C4 H41 . 109.6 no
N1 . C4 H41 . 109.6 no
C3 . C4 H42 . 109.6 no
N1 . C4 H42 . 109.6 no
H41 . C4 H42 . 109.5 no
C6 . C5 N1 . 114.50(15) yes
C6 . C5 H51 . 108.2 no
N1 . C5 H51 . 108.2 no
C6 . C5 H52 . 108.2 no
N1 . C5 H52 . 108.2 no
H51 . C5 H52 . 109.5 no
C5 . C6 C6 2_756 123.1(2) yes
C5 . C6 H61 . 118.4 no
C6 2_756 C6 H61 . 118.4 no
C8 . C7 C12 . 121.03(17) yes
C8 . C7 S1 . 116.62(14) yes
C12 . C7 S1 . 122.24(14) yes
C7 . C8 C9 . 117.58(18) yes
C7 . C8 C19 . 125.98(17) yes
C9 . C8 C19 . 116.43(18) yes
C8 . C9 C10 . 123.08(19) yes
C8 . C9 H91 . 118.4 no
C10 . C9 H91 . 118.5 no
C9 . C10 C11 . 118.10(18) yes
C9 . C10 C16 . 120.45(18) yes
C11 . C10 C16 . 121.45(19) yes
C10 . C11 C12 . 122.59(19) yes
C10 . C11 H111 . 118.7 no
C12 . C11 H111 . 118.7 no
C7 . C12 C11 . 117.45(17) yes
C7 . C12 C13 . 126.38(17) yes
C11 . C12 C13 . 116.18(18) yes
C12 . C13 C14 . 112.76(17) yes
C12 . C13 C15 . 109.96(16) yes
C14 . C13 C15 . 110.19(18) yes
C12 . C13 H131 . 108.0 no
C14 . C13 H131 . 107.9 no
C15 . C13 H131 . 107.9 no
C13 . C14 H141 . 109.5 no
C13 . C14 H142 . 109.5 no
H141 . C14 H142 . 109.5 no
C13 . C14 H143 . 109.5 no
H141 . C14 H143 . 109.5 no
H142 . C14 H143 . 109.5 no
C13 . C15 H151 . 109.5 no
C13 . C15 H152 . 109.5 no
H151 . C15 H152 . 109.5 no
C13 . C15 H153 . 109.4 no
H151 . C15 H153 . 109.5 no
H152 . C15 H153 . 109.5 no
C10 . C16 C17 . 113.4(2) yes
C10 . C16 C18 . 110.03(19) yes
C17 . C16 C18 . 110.8(2) yes
C10 . C16 H161 . 107.4 no
C17 . C16 H161 . 107.4 no
C18 . C16 H161 . 107.5 no
C16 . C17 H171 . 109.5 no
C16 . C17 H172 . 109.4 no
H171 . C17 H172 . 109.5 no
C16 . C17 H173 . 109.5 no
H171 . C17 H173 . 109.5 no
H172 . C17 H173 . 109.5 no
C16 . C18 H181 . 109.5 no
C16 . C18 H182 . 109.4 no
H181 . C18 H182 . 109.5 no
C16 . C18 H183 . 109.5 no
H181 . C18 H183 . 109.5 no
H182 . C18 H183 . 109.5 no
C8 . C19 C20 . 110.12(18) yes
C8 . C19 C21 . 111.20(19) yes
C20 . C19 C21 . 111.3(2) yes
C8 . C19 H191 . 108.0 no
C20 . C19 H191 . 108.1 no
C21 . C19 H191 . 108.1 no
C19 . C20 H201 . 109.5 no
C19 . C20 H202 . 109.5 no
H201 . C20 H202 . 109.5 no
C19 . C20 H203 . 109.4 no
H201 . C20 H203 . 109.5 no
H202 . C20 H203 . 109.5 no
C19 . C21 H211 . 109.5 no
C19 . C21 H212 . 109.4 no
H211 . C21 H212 . 109.5 no
C19 . C21 H213 . 109.5 no
H211 . C21 H213 . 109.5 no
H212 . C21 H213 . 109.5 no
C5 . N1 C4 . 115.91(14) yes
C5 . N1 S1 . 115.29(13) yes
C4 . N1 S1 . 117.86(13) yes
C7 . S1 N1 . 102.47(9) yes
C7 . S1 O1 . 108.66(10) yes
N1 . S1 O1 . 106.61(10) yes
C7 . S1 O2 . 110.35(10) yes
N1 . S1 O2 . 111.74(9) yes
O1 . S1 O2 . 116.07(10) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.483(3) yes
C1 Br1 . 1.959(3) yes
C1 H11 . 1.000 no
C1 H12 . 1.000 no
C2 C3 . 1.319(3) yes
C2 H21 . 1.000 no
C3 C4 . 1.500(3) yes
C3 H31 . 1.000 no
C4 N1 . 1.477(2) yes
C4 H41 . 1.000 no
C4 H42 . 1.000 no
C5 C6 . 1.504(3) yes
C5 N1 . 1.479(3) yes
C5 H51 . 1.000 no
C5 H52 . 1.000 no
C6 C6 2_756 1.328(4) yes
C6 H61 . 1.000 no
C7 C8 . 1.418(3) yes
C7 C12 . 1.414(3) yes
C7 S1 . 1.7916(19) yes
C8 C9 . 1.392(3) yes
C8 C19 . 1.525(3) yes
C9 C10 . 1.378(3) yes
C9 H91 . 1.000 no
C10 C11 . 1.389(3) yes
C10 C16 . 1.521(3) yes
C11 C12 . 1.402(3) yes
C11 H111 . 1.000 no
C12 C13 . 1.525(3) yes
C13 C14 . 1.524(3) yes
C13 C15 . 1.530(3) yes
C13 H131 . 1.000 no
C14 H141 . 1.000 no
C14 H142 . 1.000 no
C14 H143 . 1.000 no
C15 H151 . 1.000 no
C15 H152 . 1.000 no
C15 H153 . 1.000 no
C16 C17 . 1.507(4) yes
C16 C18 . 1.515(4) yes
C16 H161 . 1.000 no
C17 H171 . 1.000 no
C17 H172 . 1.000 no
C17 H173 . 1.000 no
C18 H181 . 1.000 no
C18 H182 . 1.000 no
C18 H183 . 1.000 no
C19 C20 . 1.529(3) yes
C19 C21 . 1.534(3) yes
C19 H191 . 1.000 no
C20 H201 . 1.000 no
C20 H202 . 1.000 no
C20 H203 . 1.000 no
C21 H211 . 1.000 no
C21 H212 . 1.000 no
C21 H213 . 1.000 no
N1 S1 . 1.6419(17) yes
O1 S1 . 1.4368(17) yes
O2 S1 . 1.4323(16) yes
