#------------------------------------------------------------------------------
#$Date: 2018-09-10 23:01:29 +0300 (Mon, 10 Sep 2018) $
#$Revision: 210797 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/28/7102802.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_7102802
loop_
_publ_author_name
'Armstrong, David R.'
'Clegg, William'
'Dale, Sophie H.'
'García-Álvarez, Joaquín'
'Harrington, Ross W.'
'Hevia, Eva'
'Honeyman, Gordon W.'
'Kennedy, Alan R.'
'Mulvey, Robert E.'
'O'Hara, Charles T.'
_publ_section_title
;
 Transamination chemistry of sodium TMP-zincate: synthesis and crystal
 structure of a chiral amidozincate
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              187
_journal_page_last               189
_journal_paper_doi               10.1039/b713987j
_journal_year                    2008
_chemical_formula_moiety         'C22 H53 N4 Na Zn'
_chemical_formula_sum            'C22 H53 N4 Na Zn'
_chemical_formula_weight         462.04
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.5662(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8591(9)
_cell_length_b                   18.6245(16)
_cell_length_c                   14.1986(12)
_cell_measurement_reflns_used    10781
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.44
_cell_volume                     2822.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7807
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1852
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0530
_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)+(0.0299P)²+14.3536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                1784
_reflns_number_total             1852
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b713987j.txt
_cod_data_source_block           rem332_compound_4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7102802
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Zn Zn 0.5000 0.62965(4) 0.7500 0.0320(3) Uani 1 2 d S . .
Na Na 0.5000 0.79244(12) 0.7500 0.0360(6) Uani 1 2 d S . .
N1 N 0.4486(4) 0.8989(2) 0.6442(3) 0.0594(12) Uani 1 1 d . A .
N2 N 0.6157(3) 0.69535(19) 0.6937(3) 0.0398(9) Uani 1 1 d . A .
C1 C 0.4534(8) 0.9608(3) 0.7084(5) 0.104(3) Uani 1 1 d U . .
H1A H 0.4646 1.0044 0.6712 0.124 Uiso 1 1 calc R A .
H1B H 0.3710 0.9648 0.7284 0.124 Uiso 1 1 calc R . .
C2 C 0.3265(6) 0.8985(4) 0.5831(5) 0.084(2) Uani 1 1 d U . .
H2A H 0.2615 0.8981 0.6227 0.126 Uiso 1 1 calc R A .
H2B H 0.3182 0.8556 0.5425 0.126 Uiso 1 1 calc R . .
H2C H 0.3171 0.9415 0.5427 0.126 Uiso 1 1 calc R . .
C3 C 0.5434(7) 0.9006(4) 0.5834(5) 0.097(2) Uani 1 1 d U . .
H3A H 0.6270 0.9005 0.6236 0.145 Uiso 1 1 calc R A .
H3B H 0.5329 0.9442 0.5440 0.145 Uiso 1 1 calc R . .
H3C H 0.5340 0.8583 0.5417 0.145 Uiso 1 1 calc R . .
C4 C 0.7375(11) 0.7147(6) 0.7666(10) 0.040(3) Uani 0.536(13) 1 d PDU A 1
H4 H 0.7058 0.7329 0.8240 0.048 Uiso 0.536(13) 1 calc PR A 1
C4A C 0.7418(15) 0.6903(9) 0.7287(10) 0.053(4) Uani 0.464(13) 1 d PDU A 2
H4A H 0.7760 0.6450 0.7059 0.063 Uiso 0.464(13) 1 calc PR A 2
C5 C 0.8199(11) 0.6511(6) 0.8047(9) 0.067(4) Uani 0.536(13) 1 d PDU A 1
H5A H 0.7677 0.6127 0.8236 0.100 Uiso 0.536(13) 1 calc PR A 1
H5B H 0.8817 0.6662 0.8604 0.100 Uiso 0.536(13) 1 calc PR A 1
H5C H 0.8634 0.6334 0.7546 0.100 Uiso 0.536(13) 1 calc PR A 1
C5A C 0.7558(11) 0.6895(8) 0.8373(9) 0.061(4) Uani 0.464(13) 1 d PDU A 2
H5A1 H 0.7120 0.6476 0.8570 0.092 Uiso 0.464(13) 1 calc PR A 2
H5A2 H 0.7196 0.7334 0.8586 0.092 Uiso 0.464(13) 1 calc PR A 2
H5A3 H 0.8449 0.6868 0.8663 0.092 Uiso 0.464(13) 1 calc PR A 2
C6 C 0.8138(19) 0.7770(8) 0.7384(11) 0.061(4) Uani 0.536(13) 1 d PDU A 1
H6A H 0.7579 0.8174 0.7166 0.092 Uiso 0.536(13) 1 calc PR A 1
H6B H 0.8565 0.7619 0.6867 0.092 Uiso 0.536(13) 1 calc PR A 1
H6C H 0.8760 0.7919 0.7940 0.092 Uiso 0.536(13) 1 calc PR A 1
C6A C 0.8134(18) 0.7548(11) 0.7014(17) 0.088(8) Uani 0.464(13) 1 d PDU A 2
H6A1 H 0.8002 0.7589 0.6315 0.132 Uiso 0.464(13) 1 calc PR A 2
H6A2 H 0.9030 0.7487 0.7268 0.132 Uiso 0.464(13) 1 calc PR A 2
H6A3 H 0.7832 0.7985 0.7283 0.132 Uiso 0.464(13) 1 calc PR A 2
C7 C 0.6151(7) 0.6909(3) 0.5912(4) 0.0758(18) Uani 1 1 d DU . .
H7A H 0.6424 0.7397 0.5738 0.091 Uiso 0.50 1 calc PR A 1
H7B H 0.6478 0.7378 0.5719 0.091 Uiso 0.50 1 d PR A 2
C8 C 0.4826(8) 0.6847(4) 0.5387(4) 0.112(3) Uani 1 1 d DU A .
H8A H 0.4818 0.6824 0.4697 0.168 Uiso 1 1 calc R . .
H8B H 0.4346 0.7265 0.5530 0.168 Uiso 1 1 calc R . .
H8C H 0.4449 0.6409 0.5592 0.168 Uiso 1 1 calc R . .
C9 C 0.723(2) 0.6396(9) 0.5732(15) 0.091(5) Uani 0.536(13) 1 d PU A 1
H9A H 0.8014 0.6534 0.6151 0.137 Uiso 0.536(13) 1 calc PR A 1
H9B H 0.7326 0.6432 0.5061 0.137 Uiso 0.536(13) 1 calc PR A 1
H9C H 0.7018 0.5900 0.5872 0.137 Uiso 0.536(13) 1 calc PR A 1
C9A C 0.668(3) 0.6213(13) 0.544(2) 0.118(8) Uani 0.464(13) 1 d PU A 2
H9D H 0.7574 0.6156 0.5696 0.178 Uiso 0.464(13) 1 calc PR A 2
H9E H 0.6557 0.6275 0.4741 0.178 Uiso 0.464(13) 1 calc PR A 2
H9F H 0.6226 0.5784 0.5586 0.178 Uiso 0.464(13) 1 calc PR A 2
C10 C 0.5000 0.5199(4) 0.7500 0.068(2) Uani 1 2 d SDU . .
C11 C 0.566(2) 0.4889(7) 0.8413(12) 0.123(6) Uani 0.50 1 d PDU A -1
H11A H 0.6539 0.5046 0.8530 0.184 Uiso 0.50 1 calc PR A -1
H11B H 0.5629 0.4364 0.8374 0.184 Uiso 0.50 1 calc PR A -1
H11C H 0.5260 0.5051 0.8939 0.184 Uiso 0.50 1 calc PR A -1
C12 C 0.555(2) 0.4896(7) 0.6649(15) 0.130(6) Uani 0.50 1 d PDU A -1
H12A H 0.5106 0.5104 0.6049 0.196 Uiso 0.50 1 calc PR A -1
H12B H 0.5458 0.4373 0.6628 0.196 Uiso 0.50 1 calc PR A -1
H12C H 0.6443 0.5020 0.6734 0.196 Uiso 0.50 1 calc PR A -1
C13 C 0.3645(10) 0.4957(7) 0.7271(14) 0.090(4) Uani 0.50 1 d PDU A -1
H13A H 0.3238 0.5167 0.6660 0.135 Uiso 0.50 1 calc PR A -1
H13B H 0.3209 0.5114 0.7781 0.135 Uiso 0.50 1 calc PR A -1
H13C H 0.3612 0.4432 0.7223 0.135 Uiso 0.50 1 calc PR A -1
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N2 Zn N2 105.4(2) . 2_656 ?
N2 Zn C10 127.28(10) . . ?
N2 Zn C10 127.28(10) 2_656 . ?
N1 Na N1 74.3(2) . 2_656 ?
N1 Na N2 117.97(14) . . ?
N1 Na N2 136.25(14) . 2_656 ?
N1 Na N2 136.24(14) 2_656 . ?
N1 Na N2 117.97(14) 2_656 2_656 ?
N1 Na C4 122.6(3) . . ?
N1 Na C4 104.4(3) 2_656 . ?
N1 Na C4 104.4(3) . 2_656 ?
N1 Na C4 122.6(3) 2_656 2_656 ?
N2 Na N2 83.26(18) . 2_656 ?
N2 Na C4 32.3(3) . . ?
N2 Na C4 96.1(3) 2_656 . ?
N2 Na C4 96.1(3) . 2_656 ?
N2 Na C4 32.3(3) 2_656 2_656 ?
C4 Na C4 120.8(5) . 2_656 ?
Na N1 C1 105.8(3) . . ?
Na N1 C2 116.0(4) . . ?
Na N1 C3 105.6(3) . . ?
C1 N1 C2 107.6(5) . . ?
C1 N1 C3 113.8(6) . . ?
C2 N1 C3 108.3(5) . . ?
Zn N2 Na 85.65(13) . . ?
Zn N2 C4 113.0(5) . . ?
Zn N2 C4A 117.8(6) . . ?
Zn N2 C7 118.1(4) . . ?
Na N2 C4 92.1(4) . . ?
Na N2 C4A 118.4(8) . . ?
Na N2 C7 117.7(3) . . ?
C4 N2 C7 121.4(6) . . ?
C4A N2 C7 100.3(7) . . ?
N1 C1 C1 117.4(5) . 2_656 ?
Na C4 N2 55.6(3) . . ?
Na C4 C5 149.8(9) . . ?
Na C4 C6 96.6(9) . . ?
N2 C4 C5 115.2(9) . . ?
N2 C4 C6 115.9(10) . . ?
C5 C4 C6 112.0(12) . . ?
N2 C4A C5A 106.0(11) . . ?
N2 C4A C6A 112.1(13) . . ?
C5A C4A C6A 107.8(14) . . ?
N2 C7 C8 109.2(5) . . ?
N2 C7 C9 109.3(9) . . ?
N2 C7 C9A 121.7(13) . . ?
C8 C7 C9 123.2(9) . . ?
C8 C7 C9A 96.4(12) . . ?
Zn C10 C11 113.0(6) . . ?
Zn C10 C12 111.3(6) . . ?
Zn C10 C13 107.3(6) . . ?
C11 C10 C12 110.2(10) . . ?
C11 C10 C13 111.6(9) . . ?
C12 C10 C13 102.9(9) . . ?
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
Zn N2 2.020(4) . ?
Zn N2 2.020(3) 2_656 ?
Zn C10 2.044(7) . ?
Na N1 2.489(4) . ?
Na N1 2.489(4) 2_656 ?
Na N2 2.419(4) . ?
Na N2 2.419(4) 2_656 ?
Na C4 2.929(11) . ?
Na C4 2.929(11) 2_656 ?
N1 C1 1.463(8) . ?
N1 C2 1.445(7) . ?
N1 C3 1.461(8) . ?
N2 C4 1.565(13) . ?
N2 C4A 1.372(16) . ?
N2 C7 1.457(6) . ?
C1 C1 1.408(12) 2_656 ?
C4 C5 1.524(11) . ?
C4 C6 1.521(11) . ?
C4A C5A 1.521(12) . ?
C4A C6A 1.520(12) . ?
C7 C8 1.498(9) . ?
C7 C9 1.568(19) . ?
C7 C9A 1.62(2) . ?
C10 C11 1.480(11) . ?
C10 C12 1.550(11) . ?
C10 C13 1.516(10) . ?
