#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:35:34 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180228 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/14/7111495.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_7111495
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-tetraphenyl-2-aza-21-carba-porphyrinato)
(bispiperidine)molybdenum(ii)
;
_chemical_name_systematic
;
(5,10,15,20-tetraphenyl-2-aza-21-carba-porphyrinato)
(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                112.359(3)
_cell_angle_beta                 94.035(3)
_cell_angle_gamma                103.615(3)
_cell_formula_units_Z            1
_cell_length_a                   9.8887(18)
_cell_length_b                   11.630(2)
_cell_length_c                   11.910(2)
_cell_measurement_reflns_used    5062
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.47
_cell_volume                     1211.5(4)
_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 0.927
_diffrn_measured_fraction_theta_max 0.927
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0482
_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            10658
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.9905
_exptl_absorpt_correction_T_min  0.7460
_exptl_absorpt_correction_type   'Empirical SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.949
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0447
_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)+(0.0564P)²+0.6891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                5107
_reflns_number_total             5580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508913asup1.cif
_cod_data_source_block           Mo(NCTPP)(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               7111495
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 1.2567(2) 0.4759(2) -0.1333(2) 0.0205(5) Uani 1 1 d .
C2 C 1.3163(3) 0.3802(2) -0.2118(2) 0.0247(5) Uani 1 1 d .
H2 H 1.3986 0.3962 -0.2464 0.030 Uiso 1 1 calc R
C3 C 1.2324(3) 0.2610(2) -0.2275(2) 0.0231(5) Uani 1 1 d .
H3 H 1.2457 0.1795 -0.2762 0.028 Uiso 1 1 calc R
C4 C 1.1219(2) 0.2805(2) -0.1581(2) 0.0200(4) Uani 1 1 d .
C5 C 1.0142(2) 0.1826(2) -0.1490(2) 0.0201(4) Uani 1 1 d .
C6 C 0.9040(2) 0.2015(2) -0.0821(2) 0.0194(4) Uani 1 1 d .
C7 C 0.7906(2) 0.1011(2) -0.0789(2) 0.0211(5) Uani 1 1 d .
H7 H 0.7799 0.0107 -0.1176 0.025 Uiso 1 1 calc R
C8 C 0.7000(3) 0.1582(2) -0.0101(2) 0.0231(5) Uani 1 1 d .
H8 H 0.6156 0.1145 0.0073 0.028 Uiso 1 1 calc R
C9 C 0.7563(2) 0.2962(2) 0.0308(2) 0.0193(4) Uani 1 1 d .
C10 C 0.6926(2) 0.3896(2) 0.0996(2) 0.0202(4) Uani 1 1 d .
C11 C 1.0160(2) 0.0457(2) -0.2210(2) 0.0223(5) Uani 1 1 d .
C12 C 1.0656(3) -0.0239(2) -0.1640(3) 0.0329(6) Uani 1 1 d .
H12 H 1.0963 0.0144 -0.0771 0.039 Uiso 1 1 calc R
C13 C 1.0706(3) -0.1484(3) -0.2322(3) 0.0393(7) Uani 1 1 d .
H13 H 1.1052 -0.1951 -0.1922 0.047 Uiso 1 1 calc R
C14 C 1.0258(3) -0.2050(2) -0.3580(3) 0.0356(7) Uani 1 1 d .
H14 H 1.0309 -0.2902 -0.4051 0.043 Uiso 1 1 calc R
C15 C 0.9740(3) -0.1381(3) -0.4148(3) 0.0389(7) Uani 1 1 d .
H15 H 0.9406 -0.1776 -0.5014 0.047 Uiso 1 1 calc R
C16 C 0.9699(3) -0.0132(3) -0.3469(2) 0.0310(6) Uani 1 1 d .
H16 H 0.9349 0.0329 -0.3876 0.037 Uiso 1 1 calc R
C17 C 0.5600(2) 0.3425(2) 0.1414(2) 0.0209(5) Uani 1 1 d .
C18 C 0.5658(3) 0.3207(3) 0.2469(3) 0.0356(6) Uani 1 1 d .
H18 H 0.6553 0.3361 0.2934 0.043 Uiso 1 1 calc R
C19 C 0.4438(3) 0.2765(3) 0.2868(3) 0.0397(7) Uani 1 1 d .
H19 H 0.4502 0.2632 0.3606 0.048 Uiso 1 1 calc R
C20 C 0.3133(3) 0.2520(2) 0.2196(3) 0.0293(6) Uani 1 1 d .
H20 H 0.2294 0.2218 0.2467 0.035 Uiso 1 1 calc R
C21 C 0.3057(3) 0.2715(2) 0.1137(3) 0.0297(6) Uani 1 1 d .
H21 H 0.2161 0.2536 0.0662 0.036 Uiso 1 1 calc R
C22 C 0.4284(3) 0.3174(2) 0.0748(2) 0.0269(5) Uani 1 1 d .
H22 H 0.4216 0.3317 0.0015 0.032 Uiso 1 1 calc R
C23 C 1.2653(3) 0.6363(2) 0.2203(2) 0.0248(5) Uani 1 1 d .
H23A H 1.2398 0.7188 0.2442 0.030 Uiso 1 1 calc R
H23B H 1.3205 0.6290 0.1530 0.030 Uiso 1 1 calc R
C24 C 1.3567(3) 0.6405(3) 0.3298(2) 0.0279(5) Uani 1 1 d .
H24A H 1.4389 0.7189 0.3606 0.033 Uiso 1 1 calc R
H24B H 1.3930 0.5636 0.3037 0.033 Uiso 1 1 calc R
C25 C 1.2743(3) 0.6426(3) 0.4329(2) 0.0308(6) Uani 1 1 d .
H25A H 1.3339 0.6382 0.5007 0.037 Uiso 1 1 calc R
H25B H 1.2475 0.7244 0.4662 0.037 Uiso 1 1 calc R
C26 C 1.1425(3) 0.5280(2) 0.3838(2) 0.0250(5) Uani 1 1 d .
H26A H 1.1700 0.4464 0.3581 0.030 Uiso 1 1 calc R
H26B H 1.0861 0.5322 0.4499 0.030 Uiso 1 1 calc R
C27 C 1.0538(2) 0.5278(2) 0.2752(2) 0.0224(5) Uani 1 1 d .
H27A H 0.9702 0.4507 0.2435 0.027 Uiso 1 1 calc R
H27B H 1.0195 0.6059 0.3031 0.027 Uiso 1 1 calc R
C28 C 0.5387(3) 1.0002(3) 0.3898(3) 0.0424(7) Uani 1 1 d .
C29 C 0.4033(3) 1.0000(3) 0.4115(3) 0.0435(7) Uani 1 1 d .
H29 H 0.3360 1.0003 0.3507 0.052 Uiso 1 1 calc R
C30 C 0.3647(3) 0.9993(3) 0.5196(3) 0.0424(7) Uani 1 1 d .
H30 H 0.2709 0.9985 0.5327 0.051 Uiso 1 1 calc R
C31 C 0.5739(6) 0.9980(6) 0.2807(5) 0.0351(12) Uani 0.50 1 d P
H31A H 0.5429 0.9086 0.2179 0.053 Uiso 0.50 1 calc PR
H31B H 0.6767 1.0320 0.2910 0.053 Uiso 0.50 1 calc PR
H31C H 0.5275 1.0517 0.2546 0.053 Uiso 0.50 1 calc PR
Mo1 Mo 1.0000 0.5000 0.0000 0.01763(10) Uani 1 2 d S
N1 N 1.1384(2) 0.41324(19) -0.10082(18) 0.0221(4) Uani 1 1 d .
N2 N 0.8817(2) 0.32028(19) -0.01317(18) 0.0217(4) Uani 1 1 d .
N3 N 1.1335(2) 0.52646(18) 0.17357(18) 0.0198(4) Uani 1 1 d .
H3A H 1.1639 0.4523 0.1523 0.024 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
N1 C1 C10 126.2(2) . 2_765
N1 C1 C2 108.5(2) . .
C10 C1 C2 125.2(2) 2_765 .
C3 C2 C1 107.3(2) . .
C3 C2 H2 126.3 . .
C1 C2 H2 126.3 . .
C2 C3 C4 108.2(2) . .
C2 C3 H3 125.9 . .
C4 C3 H3 125.9 . .
N1 C4 C5 125.7(2) . .
N1 C4 C3 108.3(2) . .
C5 C4 C3 125.9(2) . .
C6 C5 C4 126.1(2) . .
C6 C5 C11 117.5(2) . .
C4 C5 C11 116.3(2) . .
N2 C6 C5 126.1(2) . .
N2 C6 C7 108.2(2) . .
C5 C6 C7 125.7(2) . .
C8 C7 C6 108.2(2) . .
C8 C7 H7 125.9 . .
C6 C7 H7 125.9 . .
C7 C8 C9 107.4(2) . .
C7 C8 H8 126.3 . .
C9 C8 H8 126.3 . .
N2 C9 C10 126.1(2) . .
N2 C9 C8 108.2(2) . .
C10 C9 C8 125.7(2) . .
C9 C10 C1 125.7(2) . 2_765
C9 C10 C17 117.2(2) . .
C1 C10 C17 117.2(2) 2_765 .
C16 C11 C12 118.3(2) . .
C16 C11 C5 120.3(2) . .
C12 C11 C5 121.3(2) . .
C13 C12 C11 120.5(3) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C14 C13 C12 120.3(3) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C15 C14 C13 119.6(2) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C16 120.2(3) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C11 C16 C15 121.0(3) . .
C11 C16 H16 119.5 . .
C15 C16 H16 119.5 . .
C18 C17 C22 118.0(2) . .
C18 C17 C10 120.5(2) . .
C22 C17 C10 121.5(2) . .
C17 C18 C19 121.3(2) . .
C17 C18 H18 119.4 . .
C19 C18 H18 119.4 . .
C20 C19 C18 120.1(3) . .
C20 C19 H19 119.9 . .
C18 C19 H19 119.9 . .
C21 C20 C19 119.3(3) . .
C21 C20 H20 120.4 . .
C19 C20 H20 120.4 . .
C20 C21 C22 120.4(2) . .
C20 C21 H21 119.8 . .
C22 C21 H21 119.8 . .
C17 C22 C21 120.9(2) . .
C17 C22 H22 119.5 . .
C21 C22 H22 119.5 . .
N3 C23 C24 113.1(2) . .
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 . .
C23 C24 C25 111.3(2) . .
C23 C24 H24A 109.4 . .
C25 C24 H24A 109.4 . .
C23 C24 H24B 109.4 . .
C25 C24 H24B 109.4 . .
H24A C24 H24B 108.0 . .
C26 C25 C24 109.6(2) . .
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 110.9(2) . .
C27 C26 H26A 109.5 . .
C25 C26 H26A 109.5 . .
C27 C26 H26B 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 108.0 . .
N3 C27 C26 112.53(19) . .
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 . .
C31 C28 C29 119.9(4) . .
C31 C28 C30 121.6(4) . 2_676
C29 C28 C30 118.5(3) . 2_676
C30 C29 C28 120.9(3) . .
C30 C29 H29 119.6 . .
C28 C29 H29 119.6 . .
C29 C30 C28 120.7(3) . 2_676
C29 C30 H30 119.7 . .
C28 C30 H30 119.7 2_676 .
C28 C31 H31A 109.5 . .
C28 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C28 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N1 Mo1 N1 180.0 2_765 .
N1 Mo1 N2 90.09(8) 2_765 2_765
N1 Mo1 N2 89.91(8) . 2_765
N1 Mo1 N2 89.91(8) 2_765 .
N1 Mo1 N2 90.09(8) . .
N2 Mo1 N2 180.00(11) 2_765 .
N1 Mo1 N3 90.91(7) 2_765 .
N1 Mo1 N3 89.09(7) . .
N2 Mo1 N3 90.85(7) 2_765 .
N2 Mo1 N3 89.15(7) . .
N1 Mo1 N3 89.09(7) 2_765 2_765
N1 Mo1 N3 90.91(7) . 2_765
N2 Mo1 N3 89.15(7) 2_765 2_765
N2 Mo1 N3 90.85(7) . 2_765
N3 Mo1 N3 180.00(10) . 2_765
C1 N1 C4 107.64(19) . .
C1 N1 Mo1 126.07(15) . .
C4 N1 Mo1 126.03(16) . .
C9 N2 C6 107.99(18) . .
C9 N2 Mo1 125.87(15) . .
C6 N2 Mo1 125.59(16) . .
C27 N3 C23 110.44(18) . .
C27 N3 Mo1 114.16(14) . .
C23 N3 Mo1 115.91(14) . .
C27 N3 H3A 105.0 . .
C23 N3 H3A 105.0 . .
Mo1 N3 H3A 105.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.388(3) .
C1 C10 1.408(3) 2_765
C1 C2 1.434(3) .
C2 C3 1.373(3) .
C2 H2 0.9500 .
C3 C4 1.425(3) .
C3 H3 0.9500 .
C4 N1 1.392(3) .
C4 C5 1.408(3) .
C5 C6 1.404(3) .
C5 C11 1.499(3) .
C6 N2 1.392(3) .
C6 C7 1.430(3) .
C7 C8 1.372(3) .
C7 H7 0.9500 .
C8 C9 1.439(3) .
C8 H8 0.9500 .
C9 N2 1.390(3) .
C9 C10 1.402(3) .
C10 C1 1.408(3) 2_765
C10 C17 1.493(3) .
C11 C16 1.379(3) .
C11 C12 1.384(3) .
C12 C13 1.380(4) .
C12 H12 0.9500 .
C13 C14 1.376(4) .
C13 H13 0.9500 .
C14 C15 1.366(4) .
C14 H14 0.9500 .
C15 C16 1.379(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 C18 1.374(4) .
C17 C22 1.381(3) .
C18 C19 1.386(4) .
C18 H18 0.9500 .
C19 C20 1.377(4) .
C19 H19 0.9500 .
C20 C21 1.364(4) .
C20 H20 0.9500 .
C21 C22 1.390(4) .
C21 H21 0.9500 .
C22 H22 0.9500 .
C23 N3 1.488(3) .
C23 C24 1.512(3) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C25 1.517(4) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 C26 1.516(3) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 C27 1.509(3) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 N3 1.487(3) .
C27 H27A 0.9900 .
C27 H27B 0.9900 .
C28 C31 1.361(7) .
C28 C29 1.381(5) .
C28 C30 1.387(4) 2_676
C29 C30 1.371(5) .
C29 H29 0.9500 .
C30 C28 1.387(4) 2_676
C30 H30 0.9500 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
Mo1 N1 2.072(2) 2_765
Mo1 N1 2.072(2) .
Mo1 N2 2.082(2) 2_765
Mo1 N2 2.082(2) .
Mo1 N3 2.247(2) .
Mo1 N3 2.247(2) 2_765
N3 H3A 0.9300 .
