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#$Date: 2016-03-23 22:14:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179473 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/70/4337063.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_4337063
loop_
_publ_author_name
'Antoine Béziau'
'Stéphane A. Baudron'
'Audrey Fluck'
'Mir Wais Hosseini'
_publ_contact_author
; Prof Mir Wais Hosseini
  Laboratoire de Tectonique Moléculaire, 
  UMR CNRS 7140, Université de Strasbourg,
  CS 90032
  F-67081 Strasbourg Cedex, France 
;
_publ_contact_author_email       hosseini@unistra.fr
_publ_contact_author_fax         '33 3 68 85 13 23'
_publ_contact_author_phone       '33 3 68 85 13 25'
_publ_section_title
;
 From Sequential to One-Pot Synthesis of Dipyrrin Based Grid-Type Mixed
 Metal-Organic Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14439
_journal_page_last               14448
_journal_paper_doi               10.1021/ic402892f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C28 H20 N6 Pd, 2(C H4 O)'
_chemical_formula_sum            'C30 H28 N6 O2 Pd'
_chemical_formula_weight         610.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            4
_cell_length_a                   11.6653(5)
_cell_length_b                   9.7781(4)
_cell_length_c                   23.3284(9)
_cell_measurement_reflns_used    9268
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.47
_cell_volume                     2660.94(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27604
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.8974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0334
_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)+(0.0272P)²+3.5973P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                3032
_reflns_number_total             3880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402892f_si_002_05.cif
_cod_data_source_block           compound5_MeOH
_cod_database_code               4337063
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.1702(2) 0.2128(2) 0.45821(10) 0.0230(4) Uani 1 1 d .
H1 H 0.1178 0.2556 0.4341 0.028 Uiso 1 1 calc R
C2 C 0.2879(2) 0.2424(3) 0.45941(11) 0.0281(5) Uani 1 1 d .
H2 H 0.3261 0.3067 0.4371 0.034 Uiso 1 1 calc R
C3 C 0.3357(2) 0.1583(3) 0.49993(10) 0.0260(5) Uani 1 1 d .
H3 H 0.4130 0.1522 0.5094 0.031 Uiso 1 1 calc R
C4 C 0.24402(18) 0.0815(2) 0.52491(9) 0.0181(4) Uani 1 1 d .
C5 C 0.24442(19) 0.0076(2) 0.57586(9) 0.0183(4) Uani 1 1 d .
C6 C 0.14537(18) -0.0336(2) 0.60566(9) 0.0174(4) Uani 1 1 d .
C7 C 0.1379(2) -0.0641(2) 0.66516(9) 0.0211(4) Uani 1 1 d .
H7 H 0.1990 -0.0775 0.6901 0.025 Uiso 1 1 calc R
C8 C 0.0229(2) -0.0703(2) 0.67886(10) 0.0233(4) Uani 1 1 d .
H8 H -0.0084 -0.0873 0.7148 0.028 Uiso 1 1 calc R
C9 C -0.0377(2) -0.0456(2) 0.62774(10) 0.0206(4) Uani 1 1 d .
H9 H -0.1172 -0.0443 0.6247 0.025 Uiso 1 1 calc R
N2 N 0.03472(16) -0.02425(18) 0.58377(8) 0.0179(3) Uani 1 1 d .
C10 C 0.35580(18) -0.0199(2) 0.60511(9) 0.0188(4) Uani 1 1 d .
C11 C 0.3902(2) -0.1535(2) 0.61536(11) 0.0266(5) Uani 1 1 d .
H11 H 0.3454 -0.2264 0.6030 0.032 Uiso 1 1 calc R
C12 C 0.4922(2) -0.1767(2) 0.64421(12) 0.0292(5) Uani 1 1 d .
H12 H 0.5143 -0.2668 0.6507 0.035 Uiso 1 1 calc R
C13 C 0.5268(2) 0.0516(3) 0.65334(11) 0.0265(5) Uani 1 1 d .
H13 H 0.5731 0.1225 0.6663 0.032 Uiso 1 1 calc R
C14 C 0.42633(19) 0.0849(2) 0.62473(10) 0.0224(4) Uani 1 1 d .
H14 H 0.4064 0.1759 0.6188 0.027 Uiso 1 1 calc R
C15 C 0.7280(3) 0.6842(3) 0.73455(13) 0.0414(7) Uani 1 1 d .
H15A H 0.7835 0.6547 0.7623 0.062 Uiso 1 1 calc R
H15B H 0.7196 0.6152 0.7056 0.062 Uiso 1 1 calc R
H15C H 0.6556 0.6988 0.7531 0.062 Uiso 1 1 calc R
N1 N 0.14282(15) 0.11574(18) 0.49592(7) 0.0185(3) Uani 1 1 d .
N3 N 0.56059(17) -0.0768(2) 0.66327(9) 0.0278(4) Uani 1 1 d .
Pd1 Pd 0.0000 0.0000 0.5000 0.01524(7) Uani 1 2 d S
O1 O 0.76499(16) 0.8064(3) 0.70921(10) 0.0510(6) Uani 1 1 d .
H1A H 0.7108 0.8434 0.6930 0.076 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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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 C2 111.6(2) . .
N1 C1 H1 124.2 . .
C2 C1 H1 124.2 . .
C3 C2 C1 106.7(2) . .
C3 C2 H2 126.7 . .
C1 C2 H2 126.7 . .
C2 C3 C4 107.0(2) . .
C2 C3 H3 126.5 . .
C4 C3 H3 126.5 . .
C5 C4 N1 122.63(19) . .
C5 C4 C3 128.2(2) . .
N1 C4 C3 107.94(18) . .
C4 C5 C6 124.6(2) . .
C4 C5 C10 119.17(19) . .
C6 C5 C10 115.94(18) . .
N2 C6 C5 124.18(19) . .
N2 C6 C7 108.37(19) . .
C5 C6 C7 126.3(2) . .
C8 C7 C6 107.1(2) . .
C8 C7 H7 126.4 . .
C6 C7 H7 126.4 . .
C7 C8 C9 106.5(2) . .
C7 C8 H8 126.7 . .
C9 C8 H8 126.7 . .
N2 C9 C8 111.0(2) . .
N2 C9 H9 124.5 . .
C8 C9 H9 124.5 . .
C9 N2 C6 107.01(19) . .
C9 N2 Pd1 129.29(16) . .
C6 N2 Pd1 123.48(15) . .
C11 C10 C14 117.8(2) . .
C11 C10 C5 120.06(19) . .
C14 C10 C5 122.15(19) . .
C12 C11 C10 119.1(2) . .
C12 C11 H11 120.4 . .
C10 C11 H11 120.4 . .
N3 C12 C11 123.6(2) . .
N3 C12 H12 118.2 . .
C11 C12 H12 118.2 . .
N3 C13 C14 123.6(2) . .
N3 C13 H13 118.2 . .
C14 C13 H13 118.2 . .
C13 C14 C10 119.0(2) . .
C13 C14 H14 120.5 . .
C10 C14 H14 120.5 . .
O1 C15 H15A 109.5 . .
O1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
O1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C1 N1 C4 106.68(18) . .
C1 N1 Pd1 128.94(15) . .
C4 N1 Pd1 122.64(14) . .
C13 N3 C12 116.9(2) . .
N2 Pd1 N2 180.00(2) 5_556 .
N2 Pd1 N1 93.12(7) 5_556 .
N2 Pd1 N1 86.88(7) . .
N2 Pd1 N1 86.88(7) 5_556 5_556
N2 Pd1 N1 93.12(7) . 5_556
N1 Pd1 N1 180.0 . 5_556
C15 O1 H1A 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.333(3) .
C1 C2 1.404(3) .
C1 H1 0.9300 .
C2 C3 1.372(3) .
C2 H2 0.9300 .
C3 C4 1.431(3) .
C3 H3 0.9300 .
C4 C5 1.391(3) .
C4 N1 1.401(3) .
C5 C6 1.407(3) .
C5 C10 1.492(3) .
C6 N2 1.391(3) .
C6 C7 1.423(3) .
C7 C8 1.381(3) .
C7 H7 0.9300 .
C8 C9 1.407(3) .
C8 H8 0.9300 .
C9 N2 1.345(3) .
C9 H9 0.9300 .
N2 Pd1 2.0097(19) .
C10 C11 1.387(3) .
C10 C14 1.392(3) .
C11 C12 1.386(3) .
C11 H11 0.9300 .
C12 N3 1.337(3) .
C12 H12 0.9300 .
C13 N3 1.336(3) .
C13 C14 1.387(3) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 O1 1.402(4) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
N1 Pd1 2.0163(18) .
Pd1 N2 2.0097(19) 5_556
Pd1 N1 2.0163(18) 5_556
O1 H1A 0.8200 .
