#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:16:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179782 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/78/7007870.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_7007870
loop_
_publ_author_name
'Cotton, F. Albert'
'Chao, Hui'
'Murillo, Carlos A.'
'Wang, Qingsheng'
_publ_section_title
;
 A trimetal chain cocooned by two heptadentate polypyridylamide
 ligands.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5416
_journal_page_last               5422
_journal_paper_doi               10.1039/b612076h
_journal_year                    2006
_chemical_formula_moiety         C27H25N9
_chemical_formula_sum            'C27 H25 N9'
_chemical_formula_weight         475.56
_chemical_name_common            H2mpeptea
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.578(3)
_cell_length_b                   25.708(5)
_cell_length_c                   10.673(2)
_cell_measurement_reflns_used    2708
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.37
_cell_volume                     4823.1(15)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_diffrn_measurement_method       ω-scans
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7380
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_correction_T_min  0.9795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2708
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0435
_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)+(0.0623P)²+3.2624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                2327
_reflns_number_total             2708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b612076h.txt
_cod_data_source_block           cif5
_cod_original_cell_volume        4823.1(16)
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7007870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
N3 N -0.00513(9) 0.26729(6) 0.95458(17) 0.0317(4) Uani 1 1 d . . .
N5 N 0.2500 0.2500 0.9339(2) 0.0296(5) Uani 1 2 d S . .
N4 N 0.12538(9) 0.27688(7) 0.92287(16) 0.0345(4) Uani 1 1 d . . .
N2 N -0.13653(9) 0.25474(6) 0.97946(18) 0.0357(4) Uani 1 1 d . . .
H2A H -0.1794 0.2711 0.9895 0.043 Uiso 1 1 calc R . .
C53 C 0.2500 0.2500 1.1914(3) 0.0363(6) Uani 1 2 d S . .
H53A H 0.2500 0.2500 1.2795 0.044 Uiso 1 2 calc SR . .
C35 C 0.05680(10) 0.29646(7) 0.97492(18) 0.0304(4) Uani 1 1 d . . .
C33 C -0.01478(13) 0.36187(8) 1.0768(2) 0.0399(5) Uani 1 1 d . . .
H33A H -0.0181 0.3941 1.1179 0.048 Uiso 1 1 calc R . .
C52 C 0.18581(11) 0.26653(8) 1.12787(18) 0.0327(4) Uani 1 1 d . . .
H52A H 0.1426 0.2785 1.1709 0.039 Uiso 1 1 calc R . .
C32 C -0.07964(12) 0.33291(8) 1.0562(2) 0.0357(4) Uani 1 1 d . . .
H32A H -0.1275 0.3451 1.0822 0.043 Uiso 1 1 calc R . .
C51 C 0.18798(10) 0.26466(7) 0.99729(18) 0.0277(4) Uani 1 1 d . . .
C15 C -0.14340(11) 0.20218(7) 0.9500(2) 0.0332(4) Uani 1 1 d . . .
N1 N -0.21478(10) 0.18444(7) 0.96539(19) 0.0391(4) Uani 1 1 d . . .
C31 C -0.07213(11) 0.28483(8) 0.99521(19) 0.0319(4) Uani 1 1 d . . .
C14 C -0.08466(13) 0.17046(8) 0.9071(2) 0.0445(6) Uani 1 1 d . . .
H14A H -0.0352 0.1837 0.8973 0.053 Uiso 1 1 calc R . .
C34 C 0.05504(12) 0.34349(8) 1.0374(2) 0.0373(5) Uani 1 1 d . . .
H34A H 0.0999 0.3624 1.0525 0.045 Uiso 1 1 calc R . .
C13 C -0.10051(14) 0.11955(9) 0.8796(3) 0.0548(7) Uani 1 1 d . . .
H13A H -0.0616 0.0974 0.8514 0.066 Uiso 1 1 calc R . .
C12 C -0.17399(16) 0.10067(10) 0.8932(3) 0.0625(8) Uani 1 1 d . . .
H12A H -0.1861 0.0659 0.8742 0.075 Uiso 1 1 calc R . .
C11 C -0.22806(14) 0.13463(10) 0.9356(3) 0.0550(7) Uani 1 1 d . . .
H11A H -0.2780 0.1222 0.9445 0.066 Uiso 1 1 calc R . .
C4 C 0.12344(13) 0.25847(12) 0.7943(2) 0.0535(6) Uani 1 1 d . . .
H4A H 0.1736 0.2463 0.7704 0.080 Uiso 1 1 calc R . .
H4B H 0.1082 0.2867 0.7395 0.080 Uiso 1 1 calc R . .
H4C H 0.0872 0.2302 0.7873 0.080 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'
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
_geom_angle_publ_flag
C31 N3 C35 118.41(16) . . ?
C51 N5 C51 119.2(2) 14 . ?
C51 N4 C35 121.85(16) . . ?
C51 N4 C4 118.93(17) . . ?
C35 N4 C4 117.75(17) . . ?
C31 N2 C15 129.93(17) . . ?
C31 N2 H2A 115.0 . . ?
C15 N2 H2A 115.0 . . ?
C52 C53 C52 121.3(3) 14 . ?
C52 C53 H53A 119.4 14 . ?
C52 C53 H53A 119.4 . . ?
N3 C35 C34 123.38(18) . . ?
N3 C35 N4 115.35(16) . . ?
C34 C35 N4 121.23(17) . . ?
C32 C33 C34 120.1(2) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C53 C52 C51 117.2(2) . . ?
C53 C52 H52A 121.4 . . ?
C51 C52 H52A 121.4 . . ?
C33 C32 C31 118.15(19) . . ?
C33 C32 H32A 120.9 . . ?
C31 C32 H32A 120.9 . . ?
N5 C51 N4 114.79(17) . . ?
N5 C51 C52 122.50(19) . . ?
N4 C51 C52 122.70(17) . . ?
N1 C15 N2 112.47(17) . . ?
N1 C15 C14 122.22(19) . . ?
N2 C15 C14 125.30(18) . . ?
C11 N1 C15 117.23(18) . . ?
N3 C31 N2 119.66(18) . . ?
N3 C31 C32 122.12(18) . . ?
N2 C31 C32 118.20(18) . . ?
C13 C14 C15 118.6(2) . . ?
C13 C14 H14A 120.7 . . ?
C15 C14 H14A 120.7 . . ?
C33 C34 C35 117.83(19) . . ?
C33 C34 H34A 121.1 . . ?
C35 C34 H34A 121.1 . . ?
C14 C13 C12 120.1(2) . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C11 C12 C13 117.3(2) . . ?
C11 C12 H12A 121.4 . . ?
C13 C12 H12A 121.4 . . ?
N1 C11 C12 124.6(2) . . ?
N1 C11 H11A 117.7 . . ?
C12 C11 H11A 117.7 . . ?
N4 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N3 C31 1.334(3) . ?
N3 C35 1.340(2) . ?
N5 C51 1.337(2) 14 ?
N5 C51 1.337(2) . ?
N4 C51 1.393(2) . ?
N4 C35 1.420(2) . ?
N4 C4 1.451(3) . ?
N2 C31 1.381(2) . ?
N2 C15 1.393(2) . ?
N2 H2A 0.8700 . ?
C53 C52 1.383(2) 14 ?
C53 C52 1.383(2) . ?
C53 H53A 0.9400 . ?
C35 C34 1.381(3) . ?
C33 C32 1.380(3) . ?
C33 C34 1.381(3) . ?
C33 H33A 0.9400 . ?
C52 C51 1.395(3) . ?
C52 H52A 0.9400 . ?
C32 C31 1.403(3) . ?
C32 H32A 0.9400 . ?
C15 N1 1.345(3) . ?
C15 C14 1.393(3) . ?
N1 C11 1.340(3) . ?
C14 C13 1.370(3) . ?
C14 H14A 0.9400 . ?
C34 H34A 0.9400 . ?
C13 C12 1.388(4) . ?
C13 H13A 0.9400 . ?
C12 C11 1.368(4) . ?
C12 H12A 0.9400 . ?
C11 H11A 0.9400 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
