#------------------------------------------------------------------------------
#$Date: 2021-11-30 01:01:05 +0200 (Tue, 30 Nov 2021) $
#$Revision: 270916 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/93/7129328.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_7129328
loop_
_publ_author_name
'Li, Bin'
'Huse, Kevin'
'Wölper, Christoph'
'Schulz, Stephan'
_publ_section_title
;
 Synthesis and reactivity of heteroleptic zinc(i) complexes toward
 heteroallenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05617D
_journal_year                    2021
_chemical_formula_sum            'C45 H61 N5 Zn'
_chemical_formula_weight         737.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-09-22 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.356(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8458(11)
_cell_length_b                   17.2914(17)
_cell_length_c                   11.5079(11)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.17
_cell_volume                     2099.8(4)
_computing_cell_refinement       'BRUKER APEX3(v2019.1-0)'
_computing_data_collection       'BRUKER APEX3(v2019.1-0)'
_computing_data_reduction        'BRUKER APEX3(v2019.1-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'BRUKER APEX3(v2019.1-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 3/QUEEN'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            74237
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.311
_diffrn_reflns_theta_min         1.819
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       tablet
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         8327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0486P)²+0.4970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6491
_reflns_number_total             8327
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc05617d2.cif
_cod_data_source_block           lb_245m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7129328
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.961
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.75026(2) 0.250000 0.75788(2) 0.01793(5) Uani 1 2 d S T P . .
N1 N 0.56412(13) 0.250000 0.77862(12) 0.0231(3) Uani 1 2 d S T P . .
N2 N 0.85615(9) 0.33691(6) 0.83093(8) 0.01900(17) Uani 1 1 d . . . . .
N3 N 0.51355(13) 0.250000 0.66299(12) 0.0235(3) Uani 1 2 d S T P . .
N4 N 0.60508(13) 0.250000 0.60760(12) 0.0219(3) Uani 1 2 d S T P . .
C3 C 0.93996(10) 0.32376(7) 0.93368(9) 0.0197(2) Uani 1 1 d . . . . .
C4 C 0.96984(14) 0.250000 0.98366(13) 0.0202(3) Uani 1 2 d S T P . .
H4 H 1.017835 0.250000 1.063955 0.024 Uiso 1 2 calc R U P . .
C5 C 1.01270(12) 0.39050(8) 1.00142(12) 0.0288(3) Uani 1 1 d . . . . .
H5A H 1.081922 0.405141 0.964154 0.043 Uiso 1 1 calc R U . . .
H5B H 1.047726 0.375028 1.084412 0.043 Uiso 1 1 calc R U . . .
H5C H 0.955691 0.434674 0.999690 0.043 Uiso 1 1 calc R U . . .
C6 C 0.84313(11) 0.41398(7) 0.78215(10) 0.0240(2) Uani 1 1 d . . . . .
C7 C 0.92860(14) 0.44024(8) 0.71578(11) 0.0300(3) Uani 1 1 d . . . . .
C8 C 0.91203(17) 0.51455(9) 0.66744(14) 0.0423(4) Uani 1 1 d . . . . .
H8 H 0.969228 0.533271 0.622680 0.051 Uiso 1 1 calc R U . . .
C9 C 0.81388(18) 0.56160(9) 0.68340(16) 0.0485(4) Uani 1 1 d . . . . .
H9 H 0.804449 0.612121 0.650085 0.058 Uiso 1 1 calc R U . . .
C10 C 0.73035(15) 0.53510(9) 0.74739(15) 0.0433(4) Uani 1 1 d . . . . .
H10 H 0.663020 0.567649 0.757471 0.052 Uiso 1 1 calc R U . . .
C11 C 0.74220(12) 0.46104(8) 0.79822(12) 0.0307(3) Uani 1 1 d . . . . .
C12 C 1.03200(15) 0.38855(8) 0.69014(13) 0.0334(3) Uani 1 1 d . . . . .
H12 H 1.048024 0.346267 0.751069 0.040 Uiso 1 1 calc R U . . .
C13 C 1.15724(15) 0.43022(10) 0.69475(15) 0.0428(4) Uani 1 1 d . . . . .
H13A H 1.220942 0.392735 0.682771 0.064 Uiso 1 1 calc R U . . .
H13B H 1.186150 0.455184 0.772748 0.064 Uiso 1 1 calc R U . . .
H13C H 1.144965 0.469461 0.631674 0.064 Uiso 1 1 calc R U . . .
C14 C 0.9845(2) 0.35194(15) 0.5679(2) 0.0696(7) Uani 1 1 d . . . . .
H14A H 0.965458 0.392580 0.507011 0.104 Uiso 1 1 calc R U . . .
H14B H 0.907585 0.322042 0.567139 0.104 Uiso 1 1 calc R U . . .
H14C H 1.049944 0.317582 0.550664 0.104 Uiso 1 1 calc R U . . .
C15 C 0.64981(12) 0.43409(9) 0.86942(13) 0.0347(3) Uani 1 1 d . . . . .
H15 H 0.664814 0.377621 0.885474 0.042 Uiso 1 1 calc R U . . .
C16 C 0.67223(15) 0.47538(11) 0.99036(15) 0.0440(4) Uani 1 1 d . . . . .
H16A H 0.658116 0.531017 0.977466 0.066 Uiso 1 1 calc R U . . .
H16B H 0.759567 0.466393 1.034988 0.066 Uiso 1 1 calc R U . . .
H16C H 0.613348 0.455140 1.035948 0.066 Uiso 1 1 calc R U . . .
C17 C 0.51100(14) 0.44402(12) 0.80027(16) 0.0475(4) Uani 1 1 d . . . . .
H17A H 0.499120 0.419644 0.721584 0.071 Uiso 1 1 calc R U . . .
H17B H 0.490884 0.499232 0.790367 0.071 Uiso 1 1 calc R U . . .
H17C H 0.454746 0.419516 0.844901 0.071 Uiso 1 1 calc R U . . .
C18 C 0.56872(16) 0.250000 0.47614(14) 0.0231(3) Uani 1 2 d S T P . .
C19 C 0.62692(13) 0.31871(7) 0.42606(10) 0.0280(3) Uani 1 1 d . . . . .
C20 C 0.69570(13) 0.29273(9) 0.35105(11) 0.0318(3) Uani 1 1 d . . . . .
C21 C 0.42422(19) 0.250000 0.42714(18) 0.0426(5) Uani 1 2 d S T P . .
H21A H 0.404970 0.244838 0.340003 0.064 Uiso 1 2 calc R U P . .
H21B H 0.388778 0.298640 0.448652 0.064 Uiso 0.5 1 calc R U P . .
H21C H 0.386856 0.206522 0.461551 0.064 Uiso 0.5 1 calc R U P . .
C22 C 0.6045(2) 0.39965(9) 0.46145(14) 0.0498(5) Uani 1 1 d . . . . .
H22A H 0.643661 0.435913 0.415282 0.075 Uiso 1 1 calc R U . . .
H22B H 0.641893 0.406655 0.546819 0.075 Uiso 1 1 calc R U . . .
H22C H 0.513113 0.409509 0.445464 0.075 Uiso 1 1 calc R U . . .
C23 C 0.7651(2) 0.33918(14) 0.27621(14) 0.0589(6) Uani 1 1 d . . . . .
H23A H 0.732069 0.326553 0.191719 0.088 Uiso 1 1 calc R U . . .
H23B H 0.855674 0.326893 0.299202 0.088 Uiso 1 1 calc R U . . .
H23C H 0.752815 0.394430 0.288836 0.088 Uiso 1 1 calc R U . . .
C24 C 0.48145(15) 0.250000 0.85545(15) 0.0269(3) Uani 1 2 d S T P . .
C25 C 0.53771(17) 0.250000 0.97757(16) 0.0376(5) Uani 1 2 d S T P . .
H25 H 0.627457 0.250000 1.003650 0.045 Uiso 1 2 calc R U P . .
C26 C 0.4636(2) 0.250000 1.06131(18) 0.0481(6) Uani 1 2 d S T P . .
H26 H 0.502849 0.250000 1.144135 0.058 Uiso 1 2 calc R U P . .
C27 C 0.3325(2) 0.250000 1.0244(2) 0.0466(6) Uani 1 2 d S T P . .
H27 H 0.281643 0.250000 1.081398 0.056 Uiso 1 2 calc R U P . .
C28 C 0.27650(18) 0.250000 0.90308(19) 0.0384(5) Uani 1 2 d S T P . .
H28 H 0.186716 0.250000 0.877511 0.046 Uiso 1 2 calc R U P . .
C29 C 0.34901(16) 0.250000 0.81866(17) 0.0302(4) Uani 1 2 d S T P . .
H29 H 0.309069 0.250000 0.735986 0.036 Uiso 1 2 calc R U P . .
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'
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 Zn1 N2 100.19(6) . 4_565 ?
N2 Zn1 N4 128.40(3) . . ?
N2 Zn1 N4 128.40(3) 4_565 . ?
N2 Zn1 N1 115.95(3) . . ?
N2 Zn1 N1 115.95(3) 4_565 . ?
N4 Zn1 N1 61.46(5) . . ?
N3 N1 C24 117.45(13) . . ?
N3 N1 Zn1 94.16(10) . . ?
C24 N1 Zn1 148.39(11) . . ?
C3 N2 C6 119.25(10) . . ?
C3 N2 Zn1 117.48(8) . . ?
C6 N2 Zn1 123.20(7) . . ?
N4 N3 N1 108.00(13) . . ?
N3 N4 C18 116.80(13) . . ?
N3 N4 Zn1 96.38(9) . . ?
C18 N4 Zn1 146.81(11) . . ?
N2 C3 C4 124.25(11) . . ?
N2 C3 C5 119.70(11) . . ?
C4 C3 C5 116.02(10) . . ?
C3 C4 C3 130.24(14) 4_565 . ?
C7 C6 C11 120.94(12) . . ?
C7 C6 N2 119.54(11) . . ?
C11 C6 N2 119.48(12) . . ?
C8 C7 C6 118.28(14) . . ?
C8 C7 C12 119.90(14) . . ?
C6 C7 C12 121.72(12) . . ?
C9 C8 C7 121.34(17) . . ?
C10 C9 C8 119.88(15) . . ?
C9 C10 C11 121.41(15) . . ?
C10 C11 C6 118.15(15) . . ?
C10 C11 C15 120.07(13) . . ?
C6 C11 C15 121.77(13) . . ?
C7 C12 C14 108.56(15) . . ?
C7 C12 C13 114.02(13) . . ?
C14 C12 C13 109.68(13) . . ?
C11 C15 C16 111.31(13) . . ?
C11 C15 C17 112.18(14) . . ?
C16 C15 C17 110.36(12) . . ?
N4 C18 C19 110.70(9) . 4_565 ?
N4 C18 C19 110.70(9) . . ?
C19 C18 C19 102.83(15) 4_565 . ?
N4 C18 C21 112.64(15) . . ?
C19 C18 C21 109.77(9) 4_565 . ?
C19 C18 C21 109.77(9) . . ?
C20 C19 C22 129.72(14) . . ?
C20 C19 C18 108.87(12) . . ?
C22 C19 C18 121.40(13) . . ?
C19 C20 C20 109.56(8) . 4_565 ?
C19 C20 C23 128.09(16) . . ?
C20 C20 C23 122.35(11) 4_565 . ?
C25 C24 N1 116.20(15) . . ?
C25 C24 C29 118.91(16) . . ?
N1 C24 C29 124.89(16) . . ?
C26 C25 C24 120.60(17) . . ?
C27 C26 C25 120.24(19) . . ?
C26 C27 C28 119.21(19) . . ?
C29 C28 C27 121.22(17) . . ?
C28 C29 C24 119.82(17) . . ?
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
Zn1 N2 1.9591(10) . ?
Zn1 N2 1.9592(10) 4_565 ?
Zn1 N4 2.0524(13) . ?
Zn1 N1 2.0869(14) . ?
N1 N3 1.3170(18) . ?
N1 C24 1.397(2) . ?
N2 C3 1.3339(14) . ?
N2 C6 1.4402(16) . ?
N3 N4 1.298(2) . ?
N4 C18 1.473(2) . ?
C3 C4 1.4060(13) . ?
C3 C5 1.5092(17) . ?
C6 C7 1.4057(19) . ?
C6 C11 1.4101(18) . ?
C7 C8 1.395(2) . ?
C7 C12 1.515(2) . ?
C8 C9 1.385(3) . ?
C9 C10 1.372(3) . ?
C10 C11 1.401(2) . ?
C11 C15 1.507(2) . ?
C12 C14 1.520(2) . ?
C12 C13 1.528(2) . ?
C15 C16 1.533(2) . ?
C15 C17 1.5413(19) . ?
C18 C19 1.5199(17) 4_565 ?
C18 C19 1.5200(17) . ?
C18 C21 1.538(3) . ?
C19 C20 1.342(2) . ?
C19 C22 1.493(2) . ?
C20 C20 1.478(3) 4_565 ?
C20 C23 1.501(2) . ?
C24 C25 1.397(2) . ?
C24 C29 1.400(2) . ?
C25 C26 1.390(3) . ?
C26 C27 1.386(3) . ?
C27 C28 1.388(3) . ?
C28 C29 1.384(3) . ?
