#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/69/7016989.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_7016989
loop_
_publ_author_name
'Ho, Joanne H. H.'
'Wagler, Jörg'
'Willis, Anthony C.'
'Messerle, Barbara A.'
_publ_section_title
;
 Synthesis and structures of homo- and heterobimetallic rhodium(i) and/or
 iridium(i) complexes of binucleating bis(1-pyrazolyl)methane ligands.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11031
_journal_page_last               11042
_journal_paper_doi               10.1039/c1dt10499c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C28 H22 N8'
_chemical_formula_sum            'C28 H22 N8'
_chemical_formula_weight         470.54
_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                 112.0660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0732(3)
_cell_length_b                   23.3283(5)
_cell_length_c                   10.6167(3)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.63
_cell_measurement_theta_min      2.18
_cell_volume                     2312.08(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Shelx-97/ciftab(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31238
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0718P)²+0.1640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                5913
_reflns_number_total             8008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10499c.txt
_cod_data_source_block           compound1c
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7016989
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
N1 N 0.46983(9) 0.13868(4) 0.78163(9) 0.01926(18) Uani 1 1 d .
N2 N 0.59733(9) 0.11357(4) 0.85268(8) 0.01687(17) Uani 1 1 d .
N3 N 0.92022(10) 0.06517(4) 0.93709(9) 0.01990(18) Uani 1 1 d .
N4 N 0.83904(9) 0.10912(4) 0.86457(9) 0.01618(17) Uani 1 1 d .
N5 N 0.78476(10) 0.22340(4) 0.52595(9) 0.01983(18) Uani 1 1 d .
N6 N 0.80734(9) 0.18893(3) 0.43287(8) 0.01512(16) Uani 1 1 d .
N7 N 1.18225(10) 0.18957(4) 0.53016(10) 0.02196(19) Uani 1 1 d .
N8 N 1.04669(9) 0.18890(4) 0.43634(8) 0.01652(17) Uani 1 1 d .
C1 C 0.40120(12) 0.13850(5) 0.86658(12) 0.0234(2) Uani 1 1 d .
H1 H 0.3078 0.1537 0.8453 0.028 Uiso 1 1 calc R
C2 C 0.48267(13) 0.11333(5) 0.99104(12) 0.0261(2) Uani 1 1 d .
H2 H 0.4566 0.1083 1.0675 0.031 Uiso 1 1 calc R
C3 C 0.60910(12) 0.09733(5) 0.97905(11) 0.0228(2) Uani 1 1 d .
H3 H 0.6884 0.0787 1.0457 0.027 Uiso 1 1 calc R
C4 C 1.04790(12) 0.08870(5) 1.00320(11) 0.0230(2) Uani 1 1 d .
H4 H 1.1285 0.0683 1.0633 0.028 Uiso 1 1 calc R
C5 C 1.04917(13) 0.14727(5) 0.97343(13) 0.0278(2) Uani 1 1 d .
H5 H 1.1273 0.1732 1.0078 0.033 Uiso 1 1 calc R
C6 C 0.91321(12) 0.15889(5) 0.88407(12) 0.0252(2) Uani 1 1 d .
H6 H 0.8778 0.1949 0.8436 0.030 Uiso 1 1 calc R
C7 C 0.68954(11) 0.10042(4) 0.77873(10) 0.01562(18) Uani 1 1 d .
H7 H 0.6657 0.1284 0.7020 0.019 Uiso 1 1 calc R
C8 C 0.65548(12) 0.24581(5) 0.45931(12) 0.0233(2) Uani 1 1 d .
H8 H 0.6097 0.2721 0.4982 0.028 Uiso 1 1 calc R
C9 C 0.59527(12) 0.22597(5) 0.32520(12) 0.0244(2) Uani 1 1 d .
H9 H 0.5046 0.2357 0.2583 0.029 Uiso 1 1 calc R
C10 C 0.69558(11) 0.18942(5) 0.31150(10) 0.0198(2) Uani 1 1 d .
H10 H 0.6882 0.1685 0.2324 0.024 Uiso 1 1 calc R
C11 C 1.25813(13) 0.21466(5) 0.46608(13) 0.0271(2) Uani 1 1 d .
H11 H 1.3583 0.2215 0.5062 0.033 Uiso 1 1 calc R
C12 C 1.17188(13) 0.22969(5) 0.33196(13) 0.0262(2) Uani 1 1 d .
H12 H 1.2011 0.2479 0.2666 0.031 Uiso 1 1 calc R
C13 C 1.03621(12) 0.21233(5) 0.31589(11) 0.0202(2) Uani 1 1 d .
H13 H 0.9519 0.2160 0.2364 0.024 Uiso 1 1 calc R
C14 C 0.93988(10) 0.15659(4) 0.46872(10) 0.01487(18) Uani 1 1 d .
H14 H 0.9784 0.1513 0.5696 0.018 Uiso 1 1 calc R
C15 C 0.66459(10) 0.04093(4) 0.71680(10) 0.01560(19) Uani 1 1 d .
C16 C 0.59016(11) 0.00003(4) 0.75564(10) 0.0186(2) Uani 1 1 d .
H16 H 0.5542 0.0088 0.8243 0.022 Uiso 1 1 calc R
C17 C 0.56564(12) -0.05524(5) 0.69529(11) 0.0204(2) Uani 1 1 d .
H17 H 0.5132 -0.0829 0.7234 0.024 Uiso 1 1 calc R
C18 C 0.61674(11) -0.06881(4) 0.59754(11) 0.0194(2) Uani 1 1 d .
H18 H 0.6020 -0.1062 0.5595 0.023 Uiso 1 1 calc R
C19 C 0.69223(11) -0.02739(4) 0.55150(10) 0.01638(19) Uani 1 1 d .
C20 C 0.73953(11) -0.04020(4) 0.44749(10) 0.01722(19) Uani 1 1 d .
H20 H 0.7237 -0.0776 0.4091 0.021 Uiso 1 1 calc R
C21 C 0.80960(11) 0.00029(4) 0.39785(10) 0.01604(19) Uani 1 1 d .
C22 C 0.85932(11) -0.01376(4) 0.29251(10) 0.0189(2) Uani 1 1 d .
H22 H 0.8414 -0.0509 0.2528 0.023 Uiso 1 1 calc R
C23 C 0.93189(12) 0.02511(4) 0.24815(10) 0.0196(2) Uani 1 1 d .
H23 H 0.9652 0.0150 0.1784 0.023 Uiso 1 1 calc R
C24 C 0.95836(11) 0.08105(4) 0.30583(10) 0.01784(19) Uani 1 1 d .
H24 H 1.0102 0.1078 0.2744 0.021 Uiso 1 1 calc R
C25 C 0.91086(10) 0.09720(4) 0.40546(10) 0.01487(18) Uani 1 1 d .
C26 C 0.83465(10) 0.05671(4) 0.45633(9) 0.01460(18) Uani 1 1 d .
C27 C 0.78745(10) 0.06951(4) 0.56151(10) 0.01485(18) Uani 1 1 d .
H27 H 0.8038 0.1068 0.6004 0.018 Uiso 1 1 calc R
C28 C 0.71673(10) 0.02876(4) 0.61089(10) 0.01479(18) Uani 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
C1 N1 N2 104.33(9)
N1 N2 C3 112.59(9)
N1 N2 C7 117.03(8)
C3 N2 C7 129.65(9)
C4 N3 N4 104.18(9)
C6 N4 N3 112.40(9)
C6 N4 C7 126.77(9)
N3 N4 C7 120.84(8)
C8 N5 N6 104.08(8)
C10 N6 N5 112.35(8)
C10 N6 C14 127.31(8)
N5 N6 C14 120.34(8)
C11 N7 N8 104.03(9)
N7 N8 C13 112.83(9)
N7 N8 C14 117.54(8)
C13 N8 C14 128.87(9)
N1 C1 C2 111.93(10)
N1 C1 H1 124.0
C2 C1 H1 124.0
C3 C2 C1 105.16(10)
C3 C2 H2 127.4
C1 C2 H2 127.4
N2 C3 C2 105.98(10)
N2 C3 H3 127.0
C2 C3 H3 127.0
N3 C4 C5 111.81(10)
N3 C4 H4 124.1
C5 C4 H4 124.1
C6 C5 C4 104.92(10)
C6 C5 H5 127.5
C4 C5 H5 127.5
N4 C6 C5 106.70(10)
N4 C6 H6 126.7
C5 C6 H6 126.7
N4 C7 N2 110.69(8)
N4 C7 C15 111.35(8)
N2 C7 C15 113.04(8)
N4 C7 H7 107.1
N2 C7 H7 107.1
C15 C7 H7 107.1
N5 C8 C9 111.93(10)
N5 C8 H8 124.0
C9 C8 H8 124.0
C10 C9 C8 104.99(10)
C10 C9 H9 127.5
C8 C9 H9 127.5
N6 C10 C9 106.64(9)
N6 C10 H10 126.7
C9 C10 H10 126.7
N7 C11 C12 111.81(10)
N7 C11 H11 124.1
C12 C11 H11 124.1
C13 C12 C11 105.06(10)
C13 C12 H12 127.5
C11 C12 H12 127.5
N8 C13 C12 106.26(10)
N8 C13 H13 126.9
C12 C13 H13 126.9
N6 C14 N8 110.90(8)
N6 C14 C25 110.61(8)
N8 C14 C25 113.83(8)
N6 C14 H14 107.0
N8 C14 H14 107.0
C25 C14 H14 107.0
C16 C15 C28 120.04(9)
C16 C15 C7 121.85(9)
C28 C15 C7 118.07(9)
C15 C16 C17 121.27(10)
C15 C16 H16 119.4
C17 C16 H16 119.4
C18 C17 C16 120.35(10)
C18 C17 H17 119.8
C16 C17 H17 119.8
C17 C18 C19 120.56(10)
C17 C18 H18 119.7
C19 C18 H18 119.7
C20 C19 C18 120.88(9)
C20 C19 C28 119.47(9)
C18 C19 C28 119.63(9)
C19 C20 C21 121.85(9)
C19 C20 H20 119.1
C21 C20 H20 119.1
C20 C21 C22 121.17(9)
C20 C21 C26 119.24(9)
C22 C21 C26 119.57(9)
C23 C22 C21 120.89(9)
C23 C22 H22 119.6
C21 C22 H22 119.6
C22 C23 C24 120.14(10)
C22 C23 H23 119.9
C24 C23 H23 119.9
C25 C24 C23 121.45(10)
C25 C24 H24 119.3
C23 C24 H24 119.3
C24 C25 C26 119.93(9)
C24 C25 C14 121.86(9)
C26 C25 C14 118.18(8)
C27 C26 C21 118.87(9)
C27 C26 C25 123.11(9)
C21 C26 C25 118.00(9)
C26 C27 C28 121.73(9)
C26 C27 H27 119.1
C28 C27 H27 119.1
C27 C28 C19 118.84(9)
C27 C28 C15 123.03(9)
C19 C28 C15 118.12(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C1 1.3265(14)
N1 N2 1.3541(12)
N2 C3 1.3558(13)
N2 C7 1.4564(13)
N3 C4 1.3303(14)
N3 N4 1.3563(12)
N4 C6 1.3538(14)
N4 C7 1.4520(13)
N5 C8 1.3333(14)
N5 N6 1.3580(12)
N6 C10 1.3557(13)
N6 C14 1.4541(12)
N7 C11 1.3343(15)
N7 N8 1.3547(12)
N8 C13 1.3579(13)
N8 C14 1.4566(13)
C1 C2 1.3963(17)
C1 H1 0.9500
C2 C3 1.3781(16)
C2 H2 0.9500
C3 H3 0.9500
C4 C5 1.4037(17)
C4 H4 0.9500
C5 C6 1.3685(17)
C5 H5 0.9500
C6 H6 0.9500
C7 C15 1.5159(14)
C7 H7 1.0000
C8 C9 1.4002(16)
C8 H8 0.9500
C9 C10 1.3709(15)
C9 H9 0.9500
C10 H10 0.9500
C11 C12 1.4056(18)
C11 H11 0.9500
C12 C13 1.3732(16)
C12 H12 0.9500
C13 H13 0.9500
C14 C25 1.5195(14)
C14 H14 1.0000
C15 C16 1.3691(14)
C15 C28 1.4368(14)
C16 C17 1.4195(15)
C16 H16 0.9500
C17 C18 1.3578(16)
C17 H17 0.9500
C18 C19 1.4249(14)
C18 H18 0.9500
C19 C20 1.3895(15)
C19 C28 1.4344(14)
C20 C21 1.3954(14)
C20 H20 0.9500
C21 C22 1.4247(14)
C21 C26 1.4367(13)
C22 C23 1.3555(16)
C22 H22 0.9500
C23 C24 1.4236(15)
C23 H23 0.9500
C24 C25 1.3675(14)
C24 H24 0.9500
C25 C26 1.4438(14)
C26 C27 1.4004(14)
C27 C28 1.4024(14)
C27 H27 0.9500
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C1 N1 N2 C3 0.59(12)
C1 N1 N2 C7 171.75(9)
C4 N3 N4 C6 0.10(12)
C4 N3 N4 C7 -179.40(9)
C8 N5 N6 C10 -0.23(12)
C8 N5 N6 C14 179.90(9)
C11 N7 N8 C13 0.50(11)
C11 N7 N8 C14 171.42(9)
N2 N1 C1 C2 -0.33(12)
N1 C1 C2 C3 -0.03(14)
N1 N2 C3 C2 -0.62(13)
C7 N2 C3 C2 -170.38(10)
C1 C2 C3 N2 0.38(13)
N4 N3 C4 C5 -0.10(12)
N3 C4 C5 C6 0.07(14)
N3 N4 C6 C5 -0.06(13)
C7 N4 C6 C5 179.40(10)
C4 C5 C6 N4 0.00(13)
C6 N4 C7 N2 -86.37(12)
N3 N4 C7 N2 93.05(10)
C6 N4 C7 C15 146.99(10)
N3 N4 C7 C15 -33.59(12)
N1 N2 C7 N4 143.70(8)
C3 N2 C7 N4 -46.91(14)
N1 N2 C7 C15 -90.60(10)
C3 N2 C7 C15 78.79(13)
N6 N5 C8 C9 0.16(12)
N5 C8 C9 C10 -0.04(14)
N5 N6 C10 C9 0.21(12)
C14 N6 C10 C9 -179.93(10)
C8 C9 C10 N6 -0.10(13)
N8 N7 C11 C12 -0.30(12)
N7 C11 C12 C13 0.01(13)
N7 N8 C13 C12 -0.50(12)
C14 N8 C13 C12 -170.15(9)
C11 C12 C13 N8 0.28(12)
C10 N6 C14 N8 88.33(12)
N5 N6 C14 N8 -91.82(10)
C10 N6 C14 C25 -38.95(13)
N5 N6 C14 C25 140.90(9)
N7 N8 C14 N6 135.85(9)
C13 N8 C14 N6 -54.91(13)
N7 N8 C14 C25 -98.66(10)
C13 N8 C14 C25 70.58(13)
N4 C7 C15 C16 110.14(11)
N2 C7 C15 C16 -15.20(13)
N4 C7 C15 C28 -72.26(11)
N2 C7 C15 C28 162.39(8)
C28 C15 C16 C17 1.46(15)
C7 C15 C16 C17 179.01(9)
C15 C16 C17 C18 0.38(16)
C16 C17 C18 C19 -1.71(16)
C17 C18 C19 C20 -177.24(10)
C17 C18 C19 C28 1.20(15)
C18 C19 C20 C21 177.91(9)
C28 C19 C20 C21 -0.54(15)
C19 C20 C21 C22 179.07(9)
C19 C20 C21 C26 0.46(15)
C20 C21 C22 C23 -177.58(10)
C26 C21 C22 C23 1.03(15)
C21 C22 C23 C24 -0.59(15)
C22 C23 C24 C25 -0.61(15)
C23 C24 C25 C26 1.32(15)
C23 C24 C25 C14 179.35(9)
N6 C14 C25 C24 112.81(10)
N8 C14 C25 C24 -12.84(13)
N6 C14 C25 C26 -69.13(11)
N8 C14 C25 C26 165.22(8)
C20 C21 C26 C27 -0.19(14)
C22 C21 C26 C27 -178.83(9)
C20 C21 C26 C25 178.33(9)
C22 C21 C26 C25 -0.31(13)
C24 C25 C26 C27 177.61(9)
C14 C25 C26 C27 -0.49(14)
C24 C25 C26 C21 -0.85(14)
C14 C25 C26 C21 -178.95(8)
C21 C26 C27 C28 0.03(14)
C25 C26 C27 C28 -178.41(9)
C26 C27 C28 C19 -0.11(14)
C26 C27 C28 C15 -178.75(9)
C20 C19 C28 C27 0.36(14)
C18 C19 C28 C27 -178.11(9)
C20 C19 C28 C15 179.06(9)
C18 C19 C28 C15 0.60(14)
C16 C15 C28 C27 176.75(9)
C7 C15 C28 C27 -0.89(14)
C16 C15 C28 C19 -1.90(14)
C7 C15 C28 C19 -179.54(8)
