#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:43:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179489 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/86/4338692.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_4338692
loop_
_publ_author_name
'Santillan, Guillermo A.'
'Carrano, Carl J.'
_publ_section_title
;
 Cobalt, zinc, and nickel complexes of a diatopic heteroscorpionate
 ligand: building blocks for coordination polymers.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              930
_journal_page_last               939
_journal_paper_doi               10.1021/ic701718b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C76 H92 Co2 N16 O12'
_chemical_formula_weight         1539.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 114.026(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6087(8)
_cell_length_b                   19.2737(9)
_cell_length_c                   14.9969(8)
_cell_measurement_reflns_used    8825
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.69
_cell_measurement_theta_min      2.53
_cell_volume                     3856.7(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      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            69369
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         7096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0651P)²+1.4786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                5279
_reflns_number_total             7096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701718b-complex_4.cif
_cod_data_source_block           guillermo2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3856.7(3)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4338692
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Co1 Co 0.30672(2) 1.014020(16) 0.18084(2) 0.03194(12) Uani 1 1 d .
N1 N 0.34145(13) 1.10781(10) 0.13400(14) 0.0323(4) Uani 1 1 d .
N2 N 0.30790(13) 1.16901(10) 0.15650(14) 0.0312(4) Uani 1 1 d .
N3 N 0.28318(14) 1.06255(10) 0.29025(13) 0.0324(4) Uani 1 1 d .
N4 N 0.26562(13) 1.13262(10) 0.28690(13) 0.0312(4) Uani 1 1 d .
N5 N 0.91594(15) 0.77194(11) 0.19142(15) 0.0409(5) Uani 1 1 d .
N6 N 0.87209(14) 0.78407(10) 0.25575(14) 0.0353(5) Uani 1 1 d .
N7 N 0.95473(17) 0.83673(12) 0.45880(16) 0.0506(6) Uani 1 1 d .
N8 N 0.95156(15) 0.87059(10) 0.37707(16) 0.0411(5) Uani 1 1 d .
O1 O -0.18261(13) 1.08244(10) -0.17695(13) 0.0468(5) Uani 1 1 d .
O2 O 0.19254(11) 0.98412(8) 0.06206(12) 0.0361(4) Uani 1 1 d .
O3 O 0.49463(19) 1.01725(13) 0.3120(2) 0.0852(8) Uani 1 1 d .
O4 O 0.41254(15) 0.94240(12) 0.19944(18) 0.0690(6) Uani 1 1 d .
C1 C 0.4557(2) 1.07281(15) 0.0584(2) 0.0505(7) Uani 1 1 d .
H1A H 0.5273 1.0750 0.1011 0.076 Uiso 1 1 calc R
H1B H 0.4461 1.0818 -0.0091 0.076 Uiso 1 1 calc R
H1C H 0.4298 1.0266 0.0629 0.076 Uiso 1 1 calc R
C2 C 0.40070(17) 1.12635(13) 0.08969(17) 0.0373(6) Uani 1 1 d .
C3 C 0.40262(18) 1.19774(14) 0.08204(19) 0.0424(6) Uani 1 1 d .
H3 H 0.4387 1.2235 0.0528 0.051 Uiso 1 1 calc R
C4 C 0.34336(17) 1.22447(12) 0.12400(18) 0.0368(6) Uani 1 1 d .
C5 C 0.3174(2) 1.29718(13) 0.1381(2) 0.0537(7) Uani 1 1 d .
H5A H 0.2444 1.3021 0.1121 0.081 Uiso 1 1 calc R
H5B H 0.3443 1.3289 0.1037 0.081 Uiso 1 1 calc R
H5C H 0.3466 1.3083 0.2079 0.081 Uiso 1 1 calc R
C6 C 0.3332(2) 0.97059(14) 0.4140(2) 0.0540(7) Uani 1 1 d .
H6A H 0.3112 0.9403 0.3565 0.081 Uiso 1 1 calc R
H6B H 0.3002 0.9565 0.4564 0.081 Uiso 1 1 calc R
H6C H 0.4060 0.9668 0.4499 0.081 Uiso 1 1 calc R
C7 C 0.30609(19) 1.04367(13) 0.38228(18) 0.0407(6) Uani 1 1 d .
C8 C 0.3019(2) 1.10103(14) 0.4366(2) 0.0518(7) Uani 1 1 d .
H8 H 0.3146 1.1013 0.5040 0.062 Uiso 1 1 calc R
C9 C 0.2761(2) 1.15699(13) 0.37553(18) 0.0421(6) Uani 1 1 d .
C10 C 0.2633(3) 1.23106(15) 0.3945(2) 0.0632(8) Uani 1 1 d .
H10A H 0.3116 1.2592 0.3803 0.095 Uiso 1 1 calc R
H10B H 0.2748 1.2370 0.4631 0.095 Uiso 1 1 calc R
H10C H 0.1951 1.2459 0.3526 0.095 Uiso 1 1 calc R
C11 C 0.23067(16) 1.16858(12) 0.19382(16) 0.0308(5) Uani 1 1 d .
H11 H 0.2179 1.2179 0.2060 0.037 Uiso 1 1 calc R
C12 C 0.13219(16) 1.13901(11) 0.11952(16) 0.0284(5) Uani 1 1 d .
C13 C 0.10402(17) 1.15137(12) 0.02112(17) 0.0326(5) Uani 1 1 d .
H13 H 0.1478 1.1759 -0.0002 0.039 Uiso 1 1 calc R
C14 C 0.01216(17) 1.12811(12) -0.04682(17) 0.0333(5) Uani 1 1 d .
H14 H -0.0071 1.1379 -0.1141 0.040 Uiso 1 1 calc R
C15 C -0.05149(16) 1.09083(11) -0.01737(17) 0.0309(5) Uani 1 1 d .
C16 C -0.02251(17) 1.07831(13) 0.08194(18) 0.0372(6) Uani 1 1 d .
H16 H -0.0653 1.0525 0.1032 0.045 Uiso 1 1 calc R
C17 C 0.06783(17) 1.10311(12) 0.14981(18) 0.0352(6) Uani 1 1 d .
H17 H 0.0858 1.0955 0.2174 0.042 Uiso 1 1 calc R
C18 C -0.14800(17) 1.06267(12) -0.09129(18) 0.0336(5) Uani 1 1 d .
C19 C 0.9512(3) 0.67208(18) 0.1108(2) 0.0717(10) Uani 1 1 d .
H19A H 0.8965 0.6611 0.0478 0.108 Uiso 1 1 calc R
H19B H 0.9870 0.6294 0.1407 0.108 Uiso 1 1 calc R
H19C H 0.9976 0.7046 0.1008 0.108 Uiso 1 1 calc R
C20 C 0.9089(2) 0.70428(14) 0.17663(19) 0.0466(7) Uani 1 1 d .
C21 C 0.8605(2) 0.67280(14) 0.2299(2) 0.0507(7) Uani 1 1 d .
H21 H 0.8457 0.6248 0.2304 0.061 Uiso 1 1 calc R
C22 C 0.83855(19) 0.72423(13) 0.28106(18) 0.0408(6) Uani 1 1 d .
C23 C 0.7910(2) 0.72056(15) 0.3524(2) 0.0556(8) Uani 1 1 d .
H23A H 0.8227 0.7545 0.4046 0.083 Uiso 1 1 calc R
H23B H 0.7997 0.6738 0.3805 0.083 Uiso 1 1 calc R
H23C H 0.7193 0.7309 0.3188 0.083 Uiso 1 1 calc R
C24 C 1.0349(2) 0.96572(16) 0.3242(3) 0.0698(10) Uani 1 1 d .
H24A H 1.0799 1.0043 0.3564 0.105 Uiso 1 1 calc R
H24B H 0.9694 0.9840 0.2804 0.105 Uiso 1 1 calc R
H24C H 1.0633 0.9385 0.2865 0.105 Uiso 1 1 calc R
C25 C 1.02288(19) 0.92100(13) 0.3987(2) 0.0506(7) Uani 1 1 d .
C26 C 1.0752(2) 0.91745(17) 0.4978(3) 0.0668(10) Uani 1 1 d .
H26 H 1.1311 0.9452 0.5363 0.080 Uiso 1 1 calc R
C27 C 1.0310(2) 0.86545(16) 0.5319(2) 0.0599(9) Uani 1 1 d .
C28 C 1.0581(3) 0.8403(2) 0.6338(2) 0.0925(13) Uani 1 1 d .
H28A H 1.0684 0.8802 0.6774 0.139 Uiso 1 1 calc R
H28B H 1.1198 0.8129 0.6550 0.139 Uiso 1 1 calc R
H28C H 1.0037 0.8114 0.6356 0.139 Uiso 1 1 calc R
C29 C 0.87044(17) 0.85553(12) 0.28341(17) 0.0340(5) Uani 1 1 d .
H29 H 0.8839 0.8838 0.2342 0.041 Uiso 1 1 calc R
C30 C 0.76976(17) 0.87950(12) 0.27862(17) 0.0341(5) Uani 1 1 d .
C31 C 0.7658(2) 0.93063(14) 0.34212(19) 0.0441(6) Uani 1 1 d .
H31 H 0.8265 0.9460 0.3928 0.053 Uiso 1 1 calc R
C32 C 0.6775(2) 0.95961(15) 0.3341(2) 0.0482(7) Uani 1 1 d .
H32 H 0.6774 0.9962 0.3765 0.058 Uiso 1 1 calc R
C33 C 0.5900(2) 0.93580(14) 0.2650(2) 0.0478(7) Uani 1 1 d .
C34 C 0.5894(2) 0.88491(16) 0.2001(2) 0.0536(8) Uani 1 1 d .
H34 H 0.5277 0.8688 0.1517 0.064 Uiso 1 1 calc R
C35 C 0.68215(18) 0.85650(14) 0.20612(19) 0.0449(6) Uani 1 1 d .
H35 H 0.6831 0.8224 0.1608 0.054 Uiso 1 1 calc R
C36 C 0.4907(3) 0.96794(16) 0.2586(3) 0.0594(8) Uani 1 1 d .
C37 C 0.4899(3) 0.8026(2) 0.3661(3) 0.0918(13) Uani 1 1 d .
H37A H 0.5101 0.8441 0.4074 0.138 Uiso 1 1 calc R
H37B H 0.5329 0.7974 0.3305 0.138 Uiso 1 1 calc R
H37C H 0.4968 0.7616 0.4071 0.138 Uiso 1 1 calc R
O5 O 0.3928(2) 0.80912(13) 0.3013(2) 0.1008(9) Uani 1 1 d .
H4 H 0.3858 0.8462 0.2698 0.151 Uiso 1 1 calc R
C38 C 0.7518(2) 0.02602(16) 0.1263(2) 0.0575(8) Uani 1 1 d .
H38A H 0.8026 0.0579 0.1699 0.086 Uiso 1 1 calc R
H38B H 0.7066 0.0120 0.1566 0.086 Uiso 1 1 calc R
H38C H 0.7133 0.0493 0.0641 0.086 Uiso 1 1 calc R
O6 O 0.79892(15) -0.03266(10) 0.10967(15) 0.0536(5) Uani 1 1 d .
H3A H 0.8123 -0.0258 0.0610 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
O2 Co1 O4 104.23(9) . .
O2 Co1 N3 120.35(7) . .
O4 Co1 N3 125.29(9) . .
O2 Co1 N1 100.53(7) . .
O4 Co1 N1 111.45(8) . .
N3 Co1 N1 91.00(7) . .
C2 N1 N2 105.13(18) . .
C2 N1 Co1 134.28(17) . .
N2 N1 Co1 120.31(13) . .
C4 N2 N1 111.16(18) . .
C4 N2 C11 127.7(2) . .
N1 N2 C11 120.17(17) . .
C7 N3 N4 105.74(19) . .
C7 N3 Co1 131.01(17) . .
N4 N3 Co1 120.88(14) . .
C9 N4 N3 111.09(18) . .
C9 N4 C11 129.1(2) . .
N3 N4 C11 119.49(17) . .
C20 N5 N6 105.0(2) . .
C22 N6 N5 111.90(19) . .
C22 N6 C29 132.6(2) . .
N5 N6 C29 115.50(19) . .
C27 N7 N8 104.6(3) . .
C25 N8 N7 112.4(2) . .
C25 N8 C29 128.1(2) . .
N7 N8 C29 119.1(2) . .
C18 O2 Co1 104.86(14) 3_575 .
C36 O4 Co1 105.2(2) . .
N1 C2 C3 110.3(2) . .
N1 C2 C1 120.7(2) . .
C3 C2 C1 129.0(2) . .
C4 C3 C2 107.5(2) . .
N2 C4 C3 105.9(2) . .
N2 C4 C5 122.1(2) . .
C3 C4 C5 131.9(2) . .
N3 C7 C8 109.8(2) . .
N3 C7 C6 120.8(2) . .
C8 C7 C6 129.4(2) . .
C9 C8 C7 107.5(2) . .
N4 C9 C8 105.9(2) . .
N4 C9 C10 123.2(2) . .
C8 C9 C10 130.8(2) . .
N2 C11 N4 110.47(17) . .
N2 C11 C12 111.76(18) . .
N4 C11 C12 112.42(18) . .
C13 C12 C17 119.3(2) . .
C13 C12 C11 119.84(19) . .
C17 C12 C11 120.7(2) . .
C12 C13 C14 120.5(2) . .
C15 C14 C13 120.6(2) . .
C14 C15 C16 118.7(2) . .
C14 C15 C18 120.4(2) . .
C16 C15 C18 120.9(2) . .
C17 C16 C15 120.7(2) . .
C16 C17 C12 120.2(2) . .
O1 C18 O2 121.4(2) . 3_575
O1 C18 C15 121.5(2) . .
O2 C18 C15 117.1(2) 3_575 .
N5 C20 C21 110.8(2) . .
N5 C20 C19 119.8(3) . .
C21 C20 C19 129.5(3) . .
C22 C21 C20 107.1(2) . .
N6 C22 C21 105.3(2) . .
N6 C22 C23 124.2(2) . .
C21 C22 C23 130.5(2) . .
N8 C25 C26 104.9(3) . .
N8 C25 C24 123.4(3) . .
C26 C25 C24 131.7(3) . .
C25 C26 C27 107.3(3) . .
N7 C27 C26 110.8(3) . .
N7 C27 C28 119.6(3) . .
C26 C27 C28 129.6(3) . .
N6 C29 N8 111.52(19) . .
N6 C29 C30 114.04(19) . .
N8 C29 C30 112.29(19) . .
C35 C30 C31 119.2(2) . .
C35 C30 C29 120.9(2) . .
C31 C30 C29 119.6(2) . .
C32 C31 C30 122.1(3) . .
C33 C32 C31 119.5(3) . .
C32 C33 C34 120.8(3) . .
C32 C33 C36 118.8(3) . .
C34 C33 C36 120.3(3) . .
C33 C34 C35 119.6(3) . .
C30 C35 C34 118.7(3) . .
O4 C36 O3 124.3(3) . .
O4 C36 C33 117.3(3) . .
O3 C36 C33 118.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 1.9667(16) .
Co1 O4 2.005(2) .
Co1 N3 2.0359(19) .
Co1 N1 2.0757(19) .
N1 C2 1.337(3) .
N1 N2 1.371(3) .
N2 C4 1.362(3) .
N2 C11 1.449(3) .
N3 C7 1.332(3) .
N3 N4 1.372(3) .
N4 C9 1.358(3) .
N4 C11 1.452(3) .
N5 C20 1.320(3) .
N5 N6 1.378(3) .
N6 C22 1.366(3) .
N6 C29 1.441(3) .
N7 C27 1.324(4) .
N7 N8 1.373(3) .
N8 C25 1.364(3) .
N8 C29 1.451(3) .
O1 C18 1.234(3) .
O2 C18 1.289(3) 3_575
O3 C36 1.229(4) .
O4 C36 1.228(4) .
C1 C2 1.496(4) .
C2 C3 1.382(4) .
C3 C4 1.362(4) .
C4 C5 1.489(4) .
C6 C7 1.488(4) .
C7 C8 1.390(4) .
C8 C9 1.365(4) .
C9 C10 1.482(4) .
C11 C12 1.527(3) .
C12 C13 1.382(3) .
C12 C17 1.385(3) .
C13 C14 1.388(3) .
C14 C15 1.382(3) .
C15 C16 1.394(3) .
C15 C18 1.496(3) .
C16 C17 1.383(3) .
C18 O2 1.289(3) 3_575
C19 C20 1.496(4) .
C20 C21 1.402(4) .
C21 C22 1.369(4) .
C22 C23 1.496(4) .
C24 C25 1.476(5) .
C25 C26 1.368(4) .
C26 C27 1.397(5) .
C27 C28 1.494(5) .
C29 C30 1.515(3) .
C30 C35 1.373(3) .
C30 C31 1.388(3) .
C31 C32 1.365(4) .
C32 C33 1.357(4) .
C33 C34 1.379(4) .
C33 C36 1.544(4) .
C34 C35 1.430(4) .
C37 O5 1.361(4) .
C38 O6 1.398(3) .
