#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:35:34 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180228 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/14/7111496.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111496
loop_
_publ_author_name
'Harvey, John D.'
'Shaw, Janet L.'
'Herrick, Richard S.'
'Ziegler, Christopher J.'
_publ_section_title
;
 The synthesis of isostructural Mo2+ porphyrin and N-confused porphyrin
 complexes
;
_journal_issue                   37
_journal_name_full               'Chemical Communications'
_journal_page_first              4663
_journal_page_last               4665
_journal_paper_doi               10.1039/b508913a
_journal_year                    2005
_chemical_formula_sum            'C61 H58 Mo N6'
_chemical_formula_weight         971.07
_chemical_name_common
;(5,10,15,20-
tetraphenylporphyrinato)(bispiperidine)molybdenum(ii)
;
_chemical_name_systematic
;
(5,10,15,20-tetraphenylporphyrinato)(bispiperidine)molybdenum(II)
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.4130(10)
_cell_angle_beta                 93.904(2)
_cell_angle_gamma                103.4010(10)
_cell_formula_units_Z            1
_cell_length_a                   9.9529(9)
_cell_length_b                   11.6864(10)
_cell_length_c                   11.9876(11)
_cell_measurement_reflns_used    4910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.46
_cell_volume                     1234.77(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10867
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.9876
_exptl_absorpt_correction_T_min  0.8159
_exptl_absorpt_correction_type   'Empirical SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0378
_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)+(0.0353P)²+0.9801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                5308
_reflns_number_total             5671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508913asup1.cif
_cod_data_source_block           Mo(TPP)(pip)2
_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               7111496
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 1.2427(2) 0.20156(18) -0.03161(18) 0.0172(4) Uani 1 1 d .
C2 C 1.2995(2) 0.33984(19) 0.00910(19) 0.0204(4) Uani 1 1 d .
H2 H 1.3833 0.3824 -0.0088 0.024 Uiso 1 1 calc R
C3 C 1.2110(2) 0.39777(19) 0.07764(19) 0.0202(4) Uani 1 1 d .
H3 H 1.2222 0.4879 0.1158 0.024 Uiso 1 1 calc R
C4 C 1.0969(2) 0.29751(18) 0.08208(18) 0.0171(4) Uani 1 1 d .
C5 C 0.9881(2) 0.31705(18) 0.14846(18) 0.0171(4) Uani 1 1 d .
C6 C 0.8797(2) 0.22038(18) 0.15882(18) 0.0173(4) Uani 1 1 d .
C7 C 0.7697(2) 0.24160(19) 0.22864(19) 0.0212(4) Uani 1 1 d .
H7 H 0.7562 0.3228 0.2765 0.025 Uiso 1 1 calc R
C8 C 0.6869(2) 0.1224(2) 0.21372(19) 0.0221(4) Uani 1 1 d .
H8 H 0.6059 0.1067 0.2492 0.026 Uiso 1 1 calc R
C9 C 0.7454(2) 0.02694(19) 0.13507(18) 0.0176(4) Uani 1 1 d .
C10 C 0.6954(2) -0.10780(19) 0.10002(18) 0.0170(4) Uani 1 1 d .
C11 C 0.9866(2) 0.45385(18) 0.22090(19) 0.0185(4) Uani 1 1 d .
C12 C 1.0337(2) 0.5122(2) 0.3463(2) 0.0261(5) Uani 1 1 d .
H12 H 1.0692 0.4659 0.3858 0.031 Uiso 1 1 calc R
C13 C 1.0300(3) 0.6377(2) 0.4156(2) 0.0322(5) Uani 1 1 d .
H13 H 1.0636 0.6766 0.5014 0.039 Uiso 1 1 calc R
C14 C 0.9775(2) 0.7052(2) 0.3595(2) 0.0314(5) Uani 1 1 d .
H14 H 0.9732 0.7901 0.4068 0.038 Uiso 1 1 calc R
C15 C 0.9312(3) 0.6493(2) 0.2346(3) 0.0356(6) Uani 1 1 d .
H15 H 0.8959 0.6963 0.1959 0.043 Uiso 1 1 calc R
C16 C 0.9360(2) 0.5238(2) 0.1648(2) 0.0288(5) Uani 1 1 d .
H16 H 0.9046 0.4861 0.0787 0.035 Uiso 1 1 calc R
C17 C 0.5622(2) -0.15404(18) 0.14185(18) 0.0177(4) Uani 1 1 d .
C18 C 0.5673(2) -0.1712(3) 0.2501(2) 0.0318(5) Uani 1 1 d .
H18 H 0.6557 -0.1524 0.2986 0.038 Uiso 1 1 calc R
C19 C 0.4447(2) -0.2157(3) 0.2890(2) 0.0365(6) Uani 1 1 d .
H19 H 0.4501 -0.2265 0.3637 0.044 Uiso 1 1 calc R
C20 C 0.3155(2) -0.2441(2) 0.2196(2) 0.0265(5) Uani 1 1 d .
H20 H 0.2319 -0.2743 0.2460 0.032 Uiso 1 1 calc R
C21 C 0.3090(2) -0.2282(2) 0.1114(2) 0.0263(5) Uani 1 1 d .
H21 H 0.2203 -0.2483 0.0629 0.032 Uiso 1 1 calc R
C22 C 0.4314(2) -0.1828(2) 0.0723(2) 0.0232(4) Uani 1 1 d .
H22 H 0.4253 -0.1715 -0.0021 0.028 Uiso 1 1 calc R
C23 C 1.2639(2) 0.1366(2) 0.21971(19) 0.0214(4) Uani 1 1 d .
H23A H 1.2370 0.2180 0.2427 0.026 Uiso 1 1 calc R
H23B H 1.3197 0.1298 0.1533 0.026 Uiso 1 1 calc R
C24 C 1.3549(2) 0.1420(2) 0.3304(2) 0.0249(4) Uani 1 1 d .
H24A H 1.3919 0.0659 0.3053 0.030 Uiso 1 1 calc R
H24B H 1.4356 0.2202 0.3610 0.030 Uiso 1 1 calc R
C25 C 1.2713(2) 0.1441(2) 0.4329(2) 0.0265(5) Uani 1 1 d .
H25A H 1.3304 0.1414 0.5013 0.032 Uiso 1 1 calc R
H25B H 1.2425 0.2247 0.4645 0.032 Uiso 1 1 calc R
C26 C 1.1420(2) 0.0281(2) 0.38358(19) 0.0221(4) Uani 1 1 d .
H26A H 1.1714 -0.0521 0.3589 0.027 Uiso 1 1 calc R
H26B H 1.0852 0.0316 0.4489 0.027 Uiso 1 1 calc R
C27 C 1.0533(2) 0.0262(2) 0.27388(18) 0.0200(4) Uani 1 1 d .
H27A H 0.9716 -0.0513 0.2423 0.024 Uiso 1 1 calc R
H27B H 1.0174 0.1029 0.3008 0.024 Uiso 1 1 calc R
C28 C 0.6348(3) 0.5006(2) 0.4799(2) 0.0356(6) Uani 1 1 d .
H28 H 0.7279 0.5009 0.4666 0.043 Uiso 1 1 calc R
C29 C 0.5395(3) 0.5030(2) 0.3906(2) 0.0356(6) Uani 1 1 d .
C30 C 0.4040(3) 0.5024(2) 0.4124(2) 0.0375(6) Uani 1 1 d .
H30 H 0.3375 0.5040 0.3527 0.045 Uiso 1 1 calc R
C31 C 0.5756(5) 0.5031(5) 0.2807(4) 0.0312(10) Uani 0.50 1 d P
H31A H 0.5454 0.4148 0.2172 0.047 Uiso 0.50 1 calc PR
H31B H 0.6776 0.5370 0.2912 0.047 Uiso 0.50 1 calc PR
H31C H 0.5294 0.5575 0.2563 0.047 Uiso 0.50 1 calc PR
Mo1 Mo 1.0000 0.0000 0.0000 0.01425(8) Uani 1 2 d S
N1 N 1.11783(17) 0.17758(15) 0.01362(15) 0.0166(3) Uani 1 1 d .
N2 N 0.86307(17) 0.08848(15) 0.10200(15) 0.0163(3) Uani 1 1 d .
N3 N 1.13365(17) 0.02541(15) 0.17272(15) 0.0174(3) Uani 1 1 d .
H3A H 1.1649 -0.0480 0.1514 0.021 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'
Mo Mo -1.6832 0.6857 '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
C10 C1 N1 125.37(17) 2_755 .
C10 C1 C2 125.96(18) 2_755 .
N1 C1 C2 108.62(16) . .
C3 C2 C1 107.78(17) . .
C3 C2 H2 126.1 . .
C1 C2 H2 126.1 . .
C2 C3 C4 107.95(17) . .
C2 C3 H3 126.0 . .
C4 C3 H3 126.0 . .
C5 C4 N1 125.50(17) . .
C5 C4 C3 125.86(18) . .
N1 C4 C3 108.57(16) . .
C4 C5 C6 126.58(18) . .
C4 C5 C11 117.74(17) . .
C6 C5 C11 115.64(17) . .
N2 C6 C5 125.20(17) . .
N2 C6 C7 108.67(17) . .
C5 C6 C7 126.12(18) . .
C8 C7 C6 107.52(18) . .
C8 C7 H7 126.2 . .
C6 C7 H7 126.2 . .
C7 C8 C9 107.52(18) . .
C7 C8 H8 126.2 . .
C9 C8 H8 126.2 . .
N2 C9 C10 125.37(17) . .
N2 C9 C8 108.75(17) . .
C10 C9 C8 125.84(18) . .
C1 C10 C9 126.75(18) 2_755 .
C1 C10 C17 116.87(17) 2_755 .
C9 C10 C17 116.38(17) . .
C12 C11 C16 118.48(19) . .
C12 C11 C5 120.20(18) . .
C16 C11 C5 121.31(18) . .
C11 C12 C13 121.1(2) . .
C11 C12 H12 119.4 . .
C13 C12 H12 119.4 . .
C14 C13 C12 119.9(2) . .
C14 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
C13 C14 C15 119.9(2) . .
C13 C14 H14 120.0 . .
C15 C14 H14 120.0 . .
C14 C15 C16 120.3(2) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C11 C16 C15 120.3(2) . .
C11 C16 H16 119.8 . .
C15 C16 H16 119.8 . .
C18 C17 C22 118.34(19) . .
C18 C17 C10 120.47(18) . .
C22 C17 C10 121.18(18) . .
C17 C18 C19 121.0(2) . .
C17 C18 H18 119.5 . .
C19 C18 H18 119.5 . .
C20 C19 C18 120.3(2) . .
C20 C19 H19 119.9 . .
C18 C19 H19 119.9 . .
C21 C20 C19 119.3(2) . .
C21 C20 H20 120.4 . .
C19 C20 H20 120.4 . .
C20 C21 C22 120.7(2) . .
C20 C21 H21 119.6 . .
C22 C21 H21 119.6 . .
C17 C22 C21 120.3(2) . .
C17 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
N3 C23 C24 112.82(16) . .
N3 C23 H23A 109.0 . .
C24 C23 H23A 109.0 . .
N3 C23 H23B 109.0 . .
C24 C23 H23B 109.0 . .
H23A C23 H23B 107.8 . .
C25 C24 C23 111.24(17) . .
C25 C24 H24A 109.4 . .
C23 C24 H24A 109.4 . .
C25 C24 H24B 109.4 . .
C23 C24 H24B 109.4 . .
H24A C24 H24B 108.0 . .
C26 C25 C24 109.37(18) . .
C26 C25 H25A 109.8 . .
C24 C25 H25A 109.8 . .
C26 C25 H25B 109.8 . .
C24 C25 H25B 109.8 . .
H25A C25 H25B 108.2 . .
C27 C26 C25 110.81(17) . .
C27 C26 H26A 109.5 . .
C25 C26 H26A 109.5 . .
C27 C26 H26B 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 108.1 . .
N3 C27 C26 112.60(16) . .
N3 C27 H27A 109.1 . .
C26 C27 H27A 109.1 . .
N3 C27 H27B 109.1 . .
C26 C27 H27B 109.1 . .
H27A C27 H27B 107.8 . .
C30 C28 C29 121.0(2) 2_666 .
C30 C28 H28 119.5 2_666 .
C29 C28 H28 119.5 . .
C31 C29 C30 119.8(3) . .
C31 C29 C28 121.9(3) . .
C30 C29 C28 118.3(2) . .
C28 C30 C29 120.6(2) 2_666 .
C28 C30 H30 119.7 2_666 .
C29 C30 H30 119.7 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N1 Mo1 N1 180.00(8) . 2_755
N1 Mo1 N2 89.90(6) . .
N1 Mo1 N2 90.10(6) 2_755 .
N1 Mo1 N2 90.10(6) . 2_755
N1 Mo1 N2 89.90(6) 2_755 2_755
N2 Mo1 N2 180.00(9) . 2_755
N1 Mo1 N3 90.53(6) . .
N1 Mo1 N3 89.47(6) 2_755 .
N2 Mo1 N3 90.88(6) . .
N2 Mo1 N3 89.12(6) 2_755 .
N1 Mo1 N3 89.47(6) . 2_755
N1 Mo1 N3 90.53(6) 2_755 2_755
N2 Mo1 N3 89.12(6) . 2_755
N2 Mo1 N3 90.88(6) 2_755 2_755
N3 Mo1 N3 180.00(8) . 2_755
C4 N1 C1 107.08(15) . .
C4 N1 Mo1 126.27(13) . .
C1 N1 Mo1 126.26(13) . .
C6 N2 C9 107.54(15) . .
C6 N2 Mo1 126.21(13) . .
C9 N2 Mo1 126.01(13) . .
C27 N3 C23 110.44(15) . .
C27 N3 Mo1 113.71(12) . .
C23 N3 Mo1 115.56(12) . .
C27 N3 H3A 105.4 . .
C23 N3 H3A 105.4 . .
Mo1 N3 H3A 105.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C10 1.396(3) 2_755
C1 N1 1.401(2) .
C1 C2 1.452(3) .
C2 C3 1.363(3) .
C2 H2 0.9500 .
C3 C4 1.451(3) .
C3 H3 0.9500 .
C4 C5 1.397(3) .
C4 N1 1.401(2) .
C5 C6 1.420(3) .
C5 C11 1.505(3) .
C6 N2 1.390(2) .
C6 C7 1.433(3) .
C7 C8 1.382(3) .
C7 H7 0.9500 .
C8 C9 1.430(3) .
C8 H8 0.9500 .
C9 N2 1.392(2) .
C9 C10 1.417(3) .
C10 C1 1.396(3) 2_755
C10 C17 1.505(3) .
C11 C12 1.386(3) .
C11 C16 1.392(3) .
C12 C13 1.394(3) .
C12 H12 0.9500 .
C13 C14 1.376(4) .
C13 H13 0.9500 .
C14 C15 1.379(4) .
C14 H14 0.9500 .
C15 C16 1.398(3) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 C18 1.386(3) .
C17 C22 1.393(3) .
C18 C19 1.395(3) .
C18 H18 0.9500 .
C19 C20 1.379(3) .
C19 H19 0.9500 .
C20 C21 1.377(3) .
C20 H20 0.9500 .
C21 C22 1.397(3) .
C21 H21 0.9500 .
C22 H22 0.9500 .
C23 N3 1.500(2) .
C23 C24 1.527(3) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C25 1.525(3) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 C26 1.524(3) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 C27 1.523(3) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 N3 1.496(2) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C28 C30 1.383(4) 2_666
C28 C29 1.394(4) .
C28 H28 0.9500 .
C29 C31 1.389(5) .
C29 C30 1.390(4) .
C30 C28 1.383(4) 2_666
C30 H30 0.9500 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
Mo1 N1 2.0727(16) .
Mo1 N1 2.0727(16) 2_755
Mo1 N2 2.0827(16) .
Mo1 N2 2.0827(16) 2_755
Mo1 N3 2.2622(17) .
Mo1 N3 2.2622(17) 2_755
N3 H3A 0.9300 .
