#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:05:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179740 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/36/7003665.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_7003665
loop_
_publ_author_name
'Clegg, William'
'Davidson, Matthew G.'
'Graham, David V.'
'Griffen, Gemma'
'Jones, Matthew D.'
'Kennedy, Alan R.'
'O'Hara, Charles T.'
'Russo, Luca'
'Thomson, Calum M.'
_publ_section_title
;
 Synthetic and structural investigations of alkali metal diamine
 bis(phenolate) complexes
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              1295
_journal_page_last               1301
_journal_paper_doi               10.1039/b718186h
_journal_year                    2008
_chemical_formula_sum            'C52 H80 N4 Na4 O6'
_chemical_formula_weight         949.16
_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                 111.185(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2626(4)
_cell_length_b                   16.8683(6)
_cell_length_c                   21.4569(5)
_cell_measurement_reflns_used    10847
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.00
_cell_volume                     5488.3(3)
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16661
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1011P)²+8.2310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2350
_reflns_number_gt                5131
_reflns_number_total             8619
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b718186h.txt
_cod_data_source_block           dvgcoh2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7003665
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.13984(11) 0.16865(11) 0.92667(8) 0.0274(5) Uani 1 1 d . . .
Na2 Na 0.16251(11) 0.35365(11) 0.93112(8) 0.0284(5) Uani 1 1 d . A .
Na3 Na 0.33160(11) 0.24175(12) 0.99652(8) 0.0299(5) Uani 1 1 d . A .
Na4 Na 0.19756(11) 0.26369(11) 1.06763(8) 0.0265(5) Uani 1 1 d . A .
O2 O 0.1747(3) 0.4897(2) 0.90671(18) 0.0491(11) Uani 1 1 d . . .
O3 O 0.2209(2) 0.2495(2) 0.88720(14) 0.0287(8) Uani 1 1 d . A .
O4 O 0.2783(2) 0.3510(2) 1.02968(15) 0.0290(8) Uani 1 1 d . . .
O5 O 0.07893(18) 0.26807(19) 0.96811(13) 0.0232(8) Uani 1 1 d . A .
O6 O 0.25065(19) 0.15250(19) 1.02957(14) 0.0278(8) Uani 1 1 d . A .
N1 N 0.4193(3) 0.1777(3) 0.94564(19) 0.0356(11) Uani 1 1 d . . .
N2 N 0.4819(3) 0.3043(3) 1.04848(19) 0.0345(11) Uani 1 1 d . . .
N3 N 0.1017(2) 0.2068(2) 1.12011(18) 0.0278(10) Uani 1 1 d . . .
N4 N 0.2958(3) 0.2271(3) 1.17955(19) 0.0335(11) Uani 1 1 d . . .
C5 C 0.1539(5) 0.5590(4) 0.9380(3) 0.068(2) Uani 1 1 d . A .
H5A H 0.1602 0.6071 0.9137 0.082 Uiso 1 1 calc R . .
H5B H 0.1961 0.5631 0.9846 0.082 Uiso 1 1 calc R . .
C6 C 0.0627(5) 0.5545(4) 0.9378(3) 0.071(2) Uani 1 1 d . . .
H6A H 0.0515 0.6002 0.9619 0.106 Uiso 1 1 calc R A .
H6B H 0.0556 0.5055 0.9598 0.106 Uiso 1 1 calc R . .
H6C H 0.0206 0.5549 0.8916 0.106 Uiso 1 1 calc R . .
C7 C 0.2539(4) 0.4960(5) 0.8943(3) 0.072(2) Uani 1 1 d . A .
H7A H 0.2751 0.4421 0.8895 0.086 Uiso 1 1 calc R . .
H7B H 0.2993 0.5216 0.9331 0.086 Uiso 1 1 calc R . .
C8 C 0.2430(5) 0.5436(6) 0.8315(4) 0.102(3) Uani 1 1 d . . .
H8A H 0.2941 0.5348 0.8184 0.153 Uiso 1 1 calc R A .
H8B H 0.2387 0.6001 0.8405 0.153 Uiso 1 1 calc R . .
H8C H 0.1892 0.5267 0.7953 0.153 Uiso 1 1 calc R . .
C9 C 0.2459(3) 0.2575(3) 0.8349(2) 0.0267(12) Uani 1 1 d . . .
C10 C 0.1964(3) 0.3086(3) 0.7805(2) 0.0281(12) Uani 1 1 d . A .
C11 C 0.2247(3) 0.3196(3) 0.7275(2) 0.0337(13) Uani 1 1 d . . .
H11 H 0.1927 0.3551 0.6929 0.040 Uiso 1 1 calc R A .
C12 C 0.2974(3) 0.2811(4) 0.7225(2) 0.0382(14) Uani 1 1 d . A .
C13 C 0.3422(3) 0.2298(3) 0.7739(2) 0.0360(13) Uani 1 1 d . . .
H13 H 0.3925 0.2027 0.7720 0.043 Uiso 1 1 calc R A .
C14 C 0.3164(3) 0.2162(3) 0.8283(2) 0.0295(12) Uani 1 1 d . A .
C15 C 0.1127(3) 0.3461(4) 0.7795(2) 0.0401(14) Uani 1 1 d . . .
H15A H 0.1265 0.3901 0.8115 0.060 Uiso 1 1 calc R A .
H15B H 0.0771 0.3066 0.7919 0.060 Uiso 1 1 calc R . .
H15C H 0.0796 0.3662 0.7346 0.060 Uiso 1 1 calc R . .
C16 C 0.3261(4) 0.2950(4) 0.6634(3) 0.0546(18) Uani 1 1 d . . .
H16A H 0.3612 0.3437 0.6706 0.082 Uiso 1 1 calc R A .
H16B H 0.2739 0.3002 0.6225 0.082 Uiso 1 1 calc R . .
H16C H 0.3617 0.2500 0.6589 0.082 Uiso 1 1 calc R . .
C17 C 0.3638(3) 0.1517(3) 0.8774(2) 0.0357(13) Uani 1 1 d . A .
H17A H 0.3190 0.1143 0.8813 0.043 Uiso 1 1 calc R . .
H17B H 0.4016 0.1219 0.8584 0.043 Uiso 1 1 calc R . .
C18 C 0.4606(4) 0.1081(4) 0.9846(3) 0.0540(17) Uani 1 1 d . A .
H18A H 0.5033 0.0856 0.9669 0.081 Uiso 1 1 calc R . .
H18B H 0.4153 0.0685 0.9817 0.081 Uiso 1 1 calc R . .
H18C H 0.4911 0.1234 1.0314 0.081 Uiso 1 1 calc R . .
C19 C 0.4834(3) 0.2370(4) 0.9442(3) 0.0414(14) Uani 1 1 d . A .
H19A H 0.4521 0.2811 0.9146 0.050 Uiso 1 1 calc R . .
H19B H 0.5245 0.2131 0.9250 0.050 Uiso 1 1 calc R . .
C20 C 0.5369(3) 0.2706(4) 1.0139(2) 0.0448(15) Uani 1 1 d . A .
H20A H 0.5737 0.2278 1.0417 0.054 Uiso 1 1 calc R . .
H20B H 0.5770 0.3123 1.0090 0.054 Uiso 1 1 calc R . .
C21 C 0.5368(3) 0.3084(4) 1.1213(2) 0.0437(15) Uani 1 1 d . A .
H21A H 0.5567 0.2550 1.1380 0.066 Uiso 1 1 calc R . .
H21B H 0.5015 0.3304 1.1458 0.066 Uiso 1 1 calc R . .
H21C H 0.5881 0.3424 1.1280 0.066 Uiso 1 1 calc R . .
C22 C 0.4499(3) 0.3844(3) 1.0223(2) 0.0355(13) Uani 1 1 d . A .
H22A H 0.4061 0.3787 0.9764 0.043 Uiso 1 1 calc R . .
H22B H 0.5002 0.4151 1.0193 0.043 Uiso 1 1 calc R . .
C23 C 0.4083(3) 0.4316(3) 1.0627(2) 0.0298(12) Uani 1 1 d . . .
C24 C 0.4543(3) 0.4970(3) 1.0999(2) 0.0364(13) Uani 1 1 d . A .
H24 H 0.5105 0.5096 1.0984 0.044 Uiso 1 1 calc R . .
C25 C 0.4217(4) 0.5436(3) 1.1385(2) 0.0382(14) Uani 1 1 d . . .
C26 C 0.3387(3) 0.5235(3) 1.1388(2) 0.0367(13) Uani 1 1 d . A .
H26 H 0.3147 0.5544 1.1651 0.044 Uiso 1 1 calc R . .
C27 C 0.2895(3) 0.4606(3) 1.1025(2) 0.0322(13) Uani 1 1 d . . .
C28 C 0.3240(3) 0.4122(3) 1.0636(2) 0.0281(12) Uani 1 1 d . A .
C29 C 0.4721(4) 0.6139(3) 1.1786(3) 0.0538(17) Uani 1 1 d . A .
H29A H 0.5324 0.6138 1.1787 0.081 Uiso 1 1 calc R . .
H29B H 0.4738 0.6101 1.2247 0.081 Uiso 1 1 calc R . .
H29C H 0.4425 0.6632 1.1584 0.081 Uiso 1 1 calc R . .
C30 C 0.1991(3) 0.4435(3) 1.1038(3) 0.0410(14) Uani 1 1 d . A .
H30A H 0.2028 0.3996 1.1346 0.062 Uiso 1 1 calc R . .
H30B H 0.1591 0.4291 1.0588 0.062 Uiso 1 1 calc R . .
H30C H 0.1766 0.4908 1.1189 0.062 Uiso 1 1 calc R . .
C31 C -0.0025(3) 0.2686(3) 0.9673(2) 0.0221(11) Uani 1 1 d . . .
C32 C -0.0696(3) 0.3136(3) 0.9186(2) 0.0237(11) Uani 1 1 d . A .
C33 C -0.1546(3) 0.3131(3) 0.9179(2) 0.0291(12) Uani 1 1 d . . .
H33 H -0.1974 0.3443 0.8851 0.035 Uiso 1 1 calc R A .
C34 C -0.1812(3) 0.2703(3) 0.9617(2) 0.0302(12) Uani 1 1 d . A .
C35 C -0.1170(3) 0.2256(3) 1.0088(2) 0.0267(11) Uani 1 1 d . . .
H35 H -0.1331 0.1953 1.0400 0.032 Uiso 1 1 calc R A .
C36 C -0.0292(3) 0.2231(3) 1.0123(2) 0.0245(11) Uani 1 1 d . A .
C37 C 0.0346(3) 0.1681(3) 1.0619(2) 0.0263(11) Uani 1 1 d . A .
H37A H 0.0005 0.1307 1.0786 0.032 Uiso 1 1 calc R . .
H37B H 0.0655 0.1365 1.0382 0.032 Uiso 1 1 calc R . .
C38 C -0.0442(3) 0.3612(3) 0.8692(2) 0.0368(13) Uani 1 1 d . . .
H38A H -0.0964 0.3882 0.8384 0.055 Uiso 1 1 calc R A .
H38B H -0.0199 0.3258 0.8440 0.055 Uiso 1 1 calc R . .
H38C H 0.0003 0.4006 0.8931 0.055 Uiso 1 1 calc R . .
C39 C -0.2749(3) 0.2724(3) 0.9593(3) 0.0395(14) Uani 1 1 d . . .
H39A H -0.2920 0.3274 0.9631 0.059 Uiso 1 1 calc R A .
H39B H -0.2796 0.2412 0.9963 0.059 Uiso 1 1 calc R . .
H39C H -0.3141 0.2501 0.9167 0.059 Uiso 1 1 calc R . .
C40 C 0.0605(4) 0.2520(3) 1.1591(2) 0.0422(14) Uani 1 1 d . A .
H40A H 0.0254 0.2163 1.1755 0.063 Uiso 1 1 calc R . .
H40B H 0.0222 0.2929 1.1308 0.063 Uiso 1 1 calc R . .
H40C H 0.1064 0.2771 1.1971 0.063 Uiso 1 1 calc R . .
C41 C 0.1615(3) 0.1458(3) 1.1619(2) 0.0317(12) Uani 1 1 d . A .
H41A H 0.1767 0.1079 1.1325 0.038 Uiso 1 1 calc R . .
H41B H 0.1304 0.1161 1.1865 0.038 Uiso 1 1 calc R . .
C42 C 0.2467(3) 0.1806(3) 1.2121(2) 0.0383(14) Uani 1 1 d . A .
H42A H 0.2320 0.2149 1.2441 0.046 Uiso 1 1 calc R . .
H42B H 0.2845 0.1369 1.2378 0.046 Uiso 1 1 calc R . .
C43 C 0.3370(4) 0.2979(3) 1.2200(3) 0.0507(16) Uani 1 1 d . A .
H43A H 0.2914 0.3297 1.2281 0.076 Uiso 1 1 calc R . .
H43B H 0.3660 0.3298 1.1958 0.076 Uiso 1 1 calc R . .
H43C H 0.3807 0.2808 1.2628 0.076 Uiso 1 1 calc R . .
C44 C 0.3662(3) 0.1828(3) 1.1663(2) 0.0359(13) Uani 1 1 d . A .
H44A H 0.4168 0.1776 1.2090 0.043 Uiso 1 1 calc R . .
H44B H 0.3862 0.2151 1.1359 0.043 Uiso 1 1 calc R . .
C45 C 0.3431(3) 0.1016(3) 1.1362(2) 0.0342(13) Uani 1 1 d . . .
C46 C 0.3787(4) 0.0354(4) 1.1753(3) 0.0491(16) Uani 1 1 d . A .
H46 H 0.4155 0.0434 1.2207 0.059 Uiso 1 1 calc R . .
C47 C 0.3634(5) -0.0402(4) 1.1518(3) 0.067(2) Uani 1 1 d . . .
C48 C 0.3093(5) -0.0502(4) 1.0841(3) 0.0601(19) Uani 1 1 d . A .
H48 H 0.2981 -0.1022 1.0659 0.072 Uiso 1 1 calc R . .
C49 C 0.2723(4) 0.0135(3) 1.0437(2) 0.0387(14) Uani 1 1 d . . .
C50 C 0.2874(3) 0.0913(3) 1.0679(2) 0.0296(12) Uani 1 1 d . A .
C51 C 0.4010(6) -0.1120(5) 1.1958(4) 0.099(3) Uani 1 1 d . A .
H51A H 0.4313 -0.0947 1.2421 0.149 Uiso 1 1 calc R . .
H51B H 0.4429 -0.1394 1.1799 0.149 Uiso 1 1 calc R . .
H51C H 0.3530 -0.1483 1.1937 0.149 Uiso 1 1 calc R . .
C52 C 0.2133(4) -0.0004(4) 0.9707(3) 0.0543(17) Uani 1 1 d . A .
H52A H 0.2187 -0.0557 0.9586 0.082 Uiso 1 1 calc R . .
H52B H 0.2316 0.0348 0.9418 0.082 Uiso 1 1 calc R . .
H52C H 0.1518 0.0107 0.9649 0.082 Uiso 1 1 calc R . .
O1B O 0.0387(6) 0.1025(6) 0.8386(5) 0.045(3) Uiso 0.436(9) 1 d P A 2
C2B C -0.0294(9) 0.0459(9) 0.8366(7) 0.046(4) Uiso 0.436(9) 1 d P A 2
H2B1 H -0.0823 0.0526 0.7956 0.056 Uiso 0.436(9) 1 calc PR A 2
H2B2 H -0.0077 -0.0092 0.8386 0.056 Uiso 0.436(9) 1 calc PR A 2
C4B C 0.1255(12) 0.0319(12) 0.7868(10) 0.078(6) Uiso 0.436(9) 1 d P A 2
H4B1 H 0.1315 0.0226 0.7435 0.116 Uiso 0.436(9) 1 calc PR A 2
H4B2 H 0.1055 -0.0168 0.8017 0.116 Uiso 0.436(9) 1 calc PR A 2
H4B3 H 0.1827 0.0477 0.8197 0.116 Uiso 0.436(9) 1 calc PR A 2
C3B C 0.0600(10) 0.0961(9) 0.7798(7) 0.035(4) Uiso 0.436(9) 1 d P A 2
H3B1 H 0.0844 0.1471 0.7715 0.042 Uiso 0.436(9) 1 calc PR A 2
H3B2 H 0.0057 0.0848 0.7409 0.042 Uiso 0.436(9) 1 calc PR A 2
O1 O 0.0167(4) 0.0954(4) 0.8625(4) 0.036(2) Uiso 0.564(9) 1 d P A 1
C2 C -0.1341(6) 0.0816(7) 0.8587(5) 0.051(3) Uiso 0.564(9) 1 d P A 1
H2A H -0.1712 0.0519 0.8777 0.077 Uiso 0.564(9) 1 calc PR A 1
H2B H -0.1492 0.0668 0.8117 0.077 Uiso 0.564(9) 1 calc PR A 1
H2C H -0.1439 0.1386 0.8618 0.077 Uiso 0.564(9) 1 calc PR A 1
C3 C 0.0174(7) 0.0507(7) 0.8063(5) 0.044(3) Uiso 0.564(9) 1 d P A 1
H3A H -0.0410 0.0546 0.7698 0.052 Uiso 0.564(9) 1 calc PR A 1
H3B H 0.0288 -0.0058 0.8190 0.052 Uiso 0.564(9) 1 calc PR A 1
C4 C 0.0905(8) 0.0830(8) 0.7815(6) 0.044(3) Uiso 0.564(9) 1 d P A 1
H4A H 0.0844 0.0578 0.7389 0.065 Uiso 0.564(9) 1 calc PR A 1
H4B H 0.1487 0.0708 0.8148 0.065 Uiso 0.564(9) 1 calc PR A 1
H4C H 0.0841 0.1405 0.7754 0.065 Uiso 0.564(9) 1 calc PR A 1
C1 C -0.0477(4) 0.0644(4) 0.8933(3) 0.0587(17) Uiso 1 1 d . . .
H1A H -0.0937 0.0286 0.8960 0.088 Uiso 0.436(9) 1 d PR A .
H1B H -0.0684 0.1193 0.8906 0.088 Uiso 0.436(9) 1 d PR . .
H1C H 0.0056 0.0580 0.9332 0.088 Uiso 0.436(9) 1 d PR . .
H1D H -0.0417 0.0075 0.8976 0.070 Uiso 0.564(9) 1 d PR . .
H1E H -0.0321 0.0881 0.9385 0.070 Uiso 0.564(9) 1 d PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
_geom_angle_publ_flag
O3 Na1 O5 95.52(13) . . ?
O3 Na1 O1B 109.0(3) . . ?
O5 Na1 O1B 113.2(3) . . ?
O3 Na1 O6 94.03(12) . . ?
O5 Na1 O6 90.73(12) . . ?
O1B Na1 O6 144.1(3) . . ?
O3 Na1 O1 126.2(2) . . ?
O5 Na1 O1 102.6(2) . . ?
O1B Na1 O1 18.2(2) . . ?
O6 Na1 O1 135.2(2) . . ?
O4 Na2 O5 93.49(12) . . ?
O4 Na2 O3 92.28(13) . . ?
O5 Na2 O3 92.50(13) . . ?
O4 Na2 O2 96.71(14) . . ?
O5 Na2 O2 141.67(15) . . ?
O3 Na2 O2 123.74(15) . . ?
O4 Na3 O6 96.36(13) . . ?
O4 Na3 N1 152.65(17) . . ?
O6 Na3 N1 110.94(16) . . ?
O4 Na3 O3 91.48(12) . . ?
O6 Na3 O3 91.51(12) . . ?
N1 Na3 O3 86.44(13) . . ?
O4 Na3 N2 86.55(14) . . ?
O6 Na3 N2 135.77(14) . . ?
N1 Na3 N2 75.16(15) . . ?
O3 Na3 N2 132.63(14) . . ?
O5 Na4 O4 92.59(12) . . ?
O5 Na4 O6 89.61(12) . . ?
O4 Na4 O6 93.44(13) . . ?
O5 Na4 N3 88.83(12) . . ?
O4 Na4 N3 163.47(15) . . ?
O6 Na4 N3 103.05(14) . . ?
O5 Na4 N4 162.46(15) . . ?
O4 Na4 N4 104.78(14) . . ?
O6 Na4 N4 86.99(14) . . ?
N3 Na4 N4 75.23(14) . . ?
C7 O2 C5 114.2(5) . . ?
C7 O2 Na2 105.5(4) . . ?
C5 O2 Na2 128.7(4) . . ?
C9 O3 Na1 140.6(3) . . ?
C9 O3 Na2 123.6(3) . . ?
Na1 O3 Na2 85.78(12) . . ?
C9 O3 Na3 118.8(3) . . ?
Na1 O3 Na3 86.21(12) . . ?
Na2 O3 Na3 85.27(12) . . ?
C28 O4 Na3 127.3(3) . . ?
C28 O4 Na2 127.5(3) . . ?
Na3 O4 Na2 90.34(13) . . ?
C28 O4 Na4 125.5(3) . . ?
Na3 O4 Na4 85.54(13) . . ?
Na2 O4 Na4 87.40(12) . . ?
C31 O5 Na1 125.1(3) . . ?
C31 O5 Na4 120.8(2) . . ?
Na1 O5 Na4 90.09(12) . . ?
C31 O5 Na2 134.7(3) . . ?
Na1 O5 Na2 86.18(12) . . ?
Na4 O5 Na2 86.50(11) . . ?
C50 O6 Na3 121.9(3) . . ?
C50 O6 Na1 135.2(3) . . ?
Na3 O6 Na1 87.90(12) . . ?
C50 O6 Na4 123.5(3) . . ?
Na3 O6 Na4 84.62(13) . . ?
Na1 O6 Na4 88.86(12) . . ?
C19 N1 C18 112.4(4) . . ?
C19 N1 C17 111.7(4) . . ?
C18 N1 C17 108.6(4) . . ?
C19 N1 Na3 104.7(3) . . ?
C18 N1 Na3 109.6(3) . . ?
C17 N1 Na3 109.8(3) . . ?
C20 N2 C22 110.8(4) . . ?
C20 N2 C21 107.7(4) . . ?
C22 N2 C21 110.5(4) . . ?
C20 N2 Na3 106.5(3) . . ?
C22 N2 Na3 93.6(3) . . ?
C21 N2 Na3 126.7(3) . . ?
C40 N3 C41 110.7(4) . . ?
C40 N3 C37 111.3(4) . . ?
C41 N3 C37 109.1(4) . . ?
C40 N3 Na4 124.3(3) . . ?
C41 N3 Na4 99.5(3) . . ?
C37 N3 Na4 100.6(3) . . ?
C42 N4 C44 114.5(4) . . ?
C42 N4 C43 111.1(4) . . ?
C44 N4 C43 107.6(4) . . ?
C42 N4 Na4 109.2(3) . . ?
C44 N4 Na4 102.5(3) . . ?
C43 N4 Na4 111.7(3) . . ?
O2 C5 C6 111.0(5) . . ?
O2 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
O2 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C7 C8 112.6(6) . . ?
O2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
O2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C9 C14 123.3(4) . . ?
O3 C9 C10 119.5(4) . . ?
C14 C9 C10 117.1(4) . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 C15 120.2(4) . . ?
C9 C10 C15 120.3(4) . . ?
C10 C11 C12 123.1(5) . . ?
C10 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C13 C12 C11 116.8(5) . . ?
C13 C12 C16 121.8(5) . . ?
C11 C12 C16 121.3(5) . . ?
C12 C13 C14 122.5(5) . . ?
C12 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C9 C14 C13 120.8(5) . . ?
C9 C14 C17 121.2(4) . . ?
C13 C14 C17 118.0(5) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 C14 116.7(4) . . ?
N1 C17 H17A 108.1 . . ?
C14 C17 H17A 108.1 . . ?
N1 C17 H17B 108.1 . . ?
C14 C17 H17B 108.1 . . ?
H17A C17 H17B 107.3 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 C20 113.1(4) . . ?
N1 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
N1 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
N2 C20 C19 113.6(4) . . ?
N2 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
N2 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 C23 115.6(4) . . ?
N2 C22 H22A 108.4 . . ?
C23 C22 H22A 108.4 . . ?
N2 C22 H22B 108.4 . . ?
C23 C22 H22B 108.4 . . ?
H22A C22 H22B 107.4 . . ?
C24 C23 C28 119.4(5) . . ?
C24 C23 C22 119.0(5) . . ?
C28 C23 C22 121.6(4) . . ?
C25 C24 C23 123.1(5) . . ?
C25 C24 H24 118.4 . . ?
C23 C24 H24 118.4 . . ?
C24 C25 C26 116.6(5) . . ?
C24 C25 C29 122.6(5) . . ?
C26 C25 C29 120.8(5) . . ?
C27 C26 C25 123.1(5) . . ?
C27 C26 H26 118.4 . . ?
C25 C26 H26 118.4 . . ?
C26 C27 C28 119.9(5) . . ?
C26 C27 C30 120.3(5) . . ?
C28 C27 C30 119.8(5) . . ?
O4 C28 C23 121.7(5) . . ?
O4 C28 C27 120.5(4) . . ?
C23 C28 C27 117.8(5) . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O5 C31 C36 122.7(4) . . ?
O5 C31 C32 120.8(4) . . ?
C36 C31 C32 116.5(4) . . ?
C33 C32 C31 120.2(4) . . ?
C33 C32 C38 121.8(4) . . ?
C31 C32 C38 118.0(4) . . ?
C34 C33 C32 124.0(4) . . ?
C34 C33 H33 118.0 . . ?
C32 C33 H33 118.0 . . ?
C33 C34 C35 116.4(4) . . ?
C33 C34 C39 121.9(4) . . ?
C35 C34 C39 121.7(5) . . ?
C34 C35 C36 122.7(4) . . ?
C34 C35 H35 118.7 . . ?
C36 C35 H35 118.7 . . ?
C35 C36 C31 120.2(4) . . ?
C35 C36 C37 118.9(4) . . ?
C31 C36 C37 120.8(4) . . ?
N3 C37 C36 115.7(4) . . ?
N3 C37 H37A 108.4 . . ?
C36 C37 H37A 108.4 . . ?
N3 C37 H37B 108.4 . . ?
C36 C37 H37B 108.4 . . ?
H37A C37 H37B 107.4 . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N3 C40 H40A 109.5 . . ?
N3 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N3 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 C42 113.0(4) . . ?
N3 C41 H41A 109.0 . . ?
C42 C41 H41A 109.0 . . ?
N3 C41 H41B 109.0 . . ?
C42 C41 H41B 109.0 . . ?
H41A C41 H41B 107.8 . . ?
N4 C42 C41 112.3(4) . . ?
N4 C42 H42A 109.1 . . ?
C41 C42 H42A 109.1 . . ?
N4 C42 H42B 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.9 . . ?
N4 C43 H43A 109.5 . . ?
N4 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N4 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N4 C44 C45 116.9(4) . . ?
N4 C44 H44A 108.1 . . ?
C45 C44 H44A 108.1 . . ?
N4 C44 H44B 108.1 . . ?
C45 C44 H44B 108.1 . . ?
H44A C44 H44B 107.3 . . ?
C46 C45 C50 119.5(5) . . ?
C46 C45 C44 119.2(4) . . ?
C50 C45 C44 121.2(4) . . ?
C47 C46 C45 123.3(5) . . ?
C47 C46 H46 118.4 . . ?
C45 C46 H46 118.4 . . ?
C46 C47 C48 117.1(5) . . ?
C46 C47 C51 122.6(6) . . ?
C48 C47 C51 120.4(7) . . ?
C49 C48 C47 121.6(6) . . ?
C49 C48 H48 119.2 . . ?
C47 C48 H48 119.2 . . ?
C48 C49 C50 121.4(5) . . ?
C48 C49 C52 119.6(5) . . ?
C50 C49 C52 119.0(5) . . ?
O6 C50 C49 121.6(4) . . ?
O6 C50 C45 121.3(5) . . ?
C49 C50 C45 117.1(4) . . ?
C47 C51 H51A 109.5 . . ?
C47 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C47 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C3B O1B C2B 110.5(11) . . ?
C3B O1B Na1 115.7(9) . . ?
C2B O1B Na1 131.0(9) . . ?
C1 C2B O1B 103.2(11) . . ?
C1 C2B H2B1 111.1 . . ?
O1B C2B H2B1 111.1 . . ?
C1 C2B H2B2 111.1 . . ?
O1B C2B H2B2 111.1 . . ?
H2B1 C2B H2B2 109.1 . . ?
C1 C2B H1D 38.2 . . ?
O1B C2B H1D 125.8 . . ?
H2B1 C2B H1D 117.8 . . ?
H2B2 C2B H1D 73.8 . . ?
C3B C4B H4B1 109.5 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
O1B C3B C4B 111.0(12) . . ?
O1B C3B H3B1 109.4 . . ?
C4B C3B H3B1 109.4 . . ?
O1B C3B H3B2 109.4 . . ?
C4B C3B H3B2 109.4 . . ?
H3B1 C3B H3B2 108.0 . . ?
C3 O1 C1 113.7(7) . . ?
C3 O1 Na1 120.8(6) . . ?
C1 O1 Na1 120.4(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H1A 44.2 . . ?
H2A C2 H1A 67.6 . . ?
H2B C2 H1A 111.3 . . ?
H2C C2 H1A 137.4 . . ?
C1 C2 H1B 44.2 . . ?
H2A C2 H1B 125.5 . . ?
H2B C2 H1B 123.7 . . ?
H2C C2 H1B 65.3 . . ?
H1A C2 H1B 82.0 . . ?
O1 C3 C4 110.0(9) . . ?
O1 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O1 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C2 C1 C2B 94.3(8) . . ?
C2 C1 O1 115.3(7) . . ?
C2B C1 O1 45.3(6) . . ?
C2 C1 H1A 60.3 . . ?
C2B C1 H1A 108.8 . . ?
O1 C1 H1A 154.1 . . ?
C2 C1 H1B 60.1 . . ?
C2B C1 H1B 109.7 . . ?
O1 C1 H1B 85.7 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 155.8 . . ?
C2B C1 H1C 109.9 . . ?
O1 C1 H1C 83.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1D 108.2 . . ?
C2B C1 H1D 79.2 . . ?
O1 C1 H1D 108.8 . . ?
H1A C1 H1D 55.5 . . ?
H1B C1 H1D 164.9 . . ?
H1C C1 H1D 77.3 . . ?
C2 C1 H1E 107.2 . . ?
C2B C1 H1E 152.4 . . ?
O1 C1 H1E 108.3 . . ?
H1A C1 H1E 96.9 . . ?
H1B C1 H1E 68.9 . . ?
H1C C1 H1E 50.0 . . ?
H1D C1 H1E 109.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O3 2.263(4) . ?
Na1 O5 2.285(4) . ?
Na1 O1B 2.296(9) . ?
Na1 O6 2.307(3) . ?
Na1 O1 2.332(7) . ?
Na2 O4 2.268(3) . ?
Na2 O5 2.311(3) . ?
Na2 O3 2.350(4) . ?
Na2 O2 2.379(4) . ?
Na3 O4 2.259(4) . ?
Na3 O6 2.275(4) . ?
Na3 N1 2.349(4) . ?
Na3 O3 2.389(3) . ?
Na3 N2 2.522(4) . ?
Na4 O5 2.304(3) . ?
Na4 O4 2.309(4) . ?
Na4 O6 2.332(4) . ?
Na4 N3 2.427(4) . ?
Na4 N4 2.435(4) . ?
O2 C7 1.411(8) . ?
O2 C5 1.447(8) . ?
O3 C9 1.331(5) . ?
O4 C28 1.326(6) . ?
O5 C31 1.318(5) . ?
O6 C50 1.321(6) . ?
N1 C19 1.452(7) . ?
N1 C18 1.456(7) . ?
N1 C17 1.481(6) . ?
N2 C20 1.468(7) . ?
N2 C22 1.484(7) . ?
N2 C21 1.495(6) . ?
N3 C40 1.461(6) . ?
N3 C41 1.476(6) . ?
N3 C37 1.480(6) . ?
N4 C42 1.466(7) . ?
N4 C44 1.477(6) . ?
N4 C43 1.486(7) . ?
C5 C6 1.485(9) . ?
C5 H5A 0.990 . ?
C5 H5B 0.990 . ?
C6 H6A 0.980 . ?
C6 H6B 0.980 . ?
C6 H6C 0.980 . ?
C7 C8 1.523(9) . ?
C7 H7A 0.990 . ?
C7 H7B 0.990 . ?
C8 H8A 0.980 . ?
C8 H8B 0.980 . ?
C8 H8C 0.980 . ?
C9 C14 1.393(7) . ?
C9 C10 1.441(7) . ?
C10 C11 1.385(6) . ?
C10 C15 1.495(7) . ?
C11 C12 1.386(7) . ?
C11 H11 0.950 . ?
C12 C13 1.384(8) . ?
C12 C16 1.521(7) . ?
C13 C14 1.395(7) . ?
C13 H13 0.950 . ?
C14 C17 1.518(7) . ?
C15 H15A 0.980 . ?
C15 H15B 0.980 . ?
C15 H15C 0.980 . ?
C16 H16A 0.980 . ?
C16 H16B 0.980 . ?
C16 H16C 0.980 . ?
C17 H17A 0.990 . ?
C17 H17B 0.990 . ?
C18 H18A 0.980 . ?
C18 H18B 0.980 . ?
C18 H18C 0.980 . ?
C19 C20 1.540(7) . ?
C19 H19A 0.990 . ?
C19 H19B 0.990 . ?
C20 H20A 0.990 . ?
C20 H20B 0.990 . ?
C21 H21A 0.980 . ?
C21 H21B 0.980 . ?
C21 H21C 0.980 . ?
C22 C23 1.505(7) . ?
C22 H22A 0.990 . ?
C22 H22B 0.990 . ?
C23 C24 1.408(7) . ?
C23 C28 1.417(7) . ?
C24 C25 1.378(8) . ?
C24 H24 0.950 . ?
C25 C26 1.393(7) . ?
C25 C29 1.520(7) . ?
C26 C27 1.388(7) . ?
C26 H26 0.950 . ?
C27 C28 1.419(7) . ?
C27 C30 1.508(7) . ?
C29 H29A 0.980 . ?
C29 H29B 0.980 . ?
C29 H29C 0.980 . ?
C30 H30A 0.980 . ?
C30 H30B 0.980 . ?
C30 H30C 0.980 . ?
C31 C36 1.419(7) . ?
C31 C32 1.427(6) . ?
C32 C33 1.377(6) . ?
C32 C38 1.500(7) . ?
C33 C34 1.374(7) . ?
C33 H33 0.950 . ?
C34 C35 1.385(7) . ?
C34 C39 1.505(6) . ?
C35 C36 1.405(6) . ?
C35 H35 0.950 . ?
C36 C37 1.507(6) . ?
C37 H37A 0.990 . ?
C37 H37B 0.990 . ?
C38 H38A 0.980 . ?
C38 H38B 0.980 . ?
C38 H38C 0.980 . ?
C39 H39A 0.980 . ?
C39 H39B 0.980 . ?
C39 H39C 0.980 . ?
C40 H40A 0.980 . ?
C40 H40B 0.980 . ?
C40 H40C 0.980 . ?
C41 C42 1.532(7) . ?
C41 H41A 0.990 . ?
C41 H41B 0.990 . ?
C42 H42A 0.990 . ?
C42 H42B 0.990 . ?
C43 H43A 0.980 . ?
C43 H43B 0.980 . ?
C43 H43C 0.980 . ?
C44 C45 1.503(8) . ?
C44 H44A 0.990 . ?
C44 H44B 0.990 . ?
C45 C46 1.390(8) . ?
C45 C50 1.429(7) . ?
C46 C47 1.361(9) . ?
C46 H46 0.950 . ?
C47 C48 1.412(8) . ?
C47 C51 1.521(9) . ?
C48 C49 1.374(7) . ?
C48 H48 0.950 . ?
C49 C50 1.399(7) . ?
C49 C52 1.531(7) . ?
C51 H51A 0.980 . ?
C51 H51B 0.980 . ?
C51 H51C 0.980 . ?
C52 H52A 0.980 . ?
C52 H52B 0.980 . ?
C52 H52C 0.980 . ?
O1B C3B 1.430(17) . ?
O1B C2B 1.451(18) . ?
C2B C1 1.388(14) . ?
C2B H2B1 0.990 . ?
C2B H2B2 0.990 . ?
C2B H1D 1.5360 . ?
C4B C3B 1.49(2) . ?
C4B H4B1 0.980 . ?
C4B H4B2 0.980 . ?
C4B H4B3 0.980 . ?
C3B H3B1 0.990 . ?
C3B H3B2 0.990 . ?
O1 C3 1.425(14) . ?
O1 C1 1.519(10) . ?
C2 C1 1.362(11) . ?
C2 H2A 0.980 . ?
C2 H2B 0.980 . ?
C2 H2C 0.980 . ?
C2 H1A 1.2218 . ?
C2 H1B 1.2183 . ?
C3 C4 1.565(15) . ?
C3 H3A 0.990 . ?
C3 H3B 0.990 . ?
C4 H4A 0.980 . ?
C4 H4B 0.980 . ?
C4 H4C 0.980 . ?
C1 H1A 0.980 . ?
C1 H1B 0.980 . ?
C1 H1C 0.980 . ?
C1 H1D 0.9668 . ?
C1 H1E 0.9929 . ?
