#------------------------------------------------------------------------------
#$Date: 2022-05-18 01:09:21 +0300 (Wed, 18 May 2022) $
#$Revision: 275491 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/69/1566990.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_1566990
loop_
_publ_author_name
'Amdur, Moses J.'
'Mullin, Kathleen'
'Waters, Michael'
'Puggioni, Danilo'
'Wojnar, Michael'
'Gu, Mingqiang'
'Sun, Lei'
'Oyala, Paul'
'Rondinelli, James'
'Freedman, Danna'
_publ_section_title
;
 Chemical Control of Spin-Lattice Relaxation to Create a Room Temperature
 Molecular Qubit
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06130E
_journal_year                    2022
_chemical_formula_moiety         'C14 H26 N4 Zn'
_chemical_formula_sum            'C14 H26 N4 Zn'
_chemical_formula_weight         315.76
_chemical_name_systematic        'Zinc Bis(N,N'-Dimethyl-4-penten-2-amine)'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2021-08-16 deposited with the CCDC.	2022-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0640(4)
_cell_length_b                   11.9661(5)
_cell_length_c                   10.8780(3)
_cell_measurement_reflns_used    6148
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      35.2420
_cell_measurement_theta_min      2.3790
_cell_volume                     1570.34(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  66.00   0.50    6.00    --   18.37  77.00   0.00  138
  2  ω     -1.00  43.00   0.50    6.00    --   18.37  -2.00 170.00   88
  3  ω     33.00  70.00   0.50    6.00    --   18.37-134.00 137.00   74
  4  ω    -55.00  13.00   0.50    6.00    --   18.37 -37.00-180.00  136
  5  ω    -71.00 -46.00   0.50    6.00    --  -18.84 138.00 -68.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0580286000
_diffrn_orient_matrix_UB_12      -0.0097313000
_diffrn_orient_matrix_UB_13      0.0004104000
_diffrn_orient_matrix_UB_21      0.0095951000
_diffrn_orient_matrix_UB_22      -0.0584691000
_diffrn_orient_matrix_UB_23      0.0017300000
_diffrn_orient_matrix_UB_31      -0.0000083000
_diffrn_orient_matrix_UB_32      0.0014840000
_diffrn_orient_matrix_UB_33      0.0651396000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13850
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.736
_diffrn_reflns_theta_min         2.397
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0364P)²+0.3547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2531
_reflns_number_total             3287
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc06130e2.cif
_cod_data_source_block           znme2nac
_cod_database_code               1566990
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         ZnC14N4H26
_chemical_oxdiff_usercomment     NoTwin
_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.
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C006(H00A,H00B,H00C), C008(H00D,H00E,H00F), C009(H00G,H00H,H00I), C00A(H00J,
 H00K,H00L)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.549
_oxdiff_exptl_absorpt_empirical_full_min 0.598
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, 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_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
Zn01 Zn 0.500000 0.36848(2) 0.250000 0.01290(6) Uani 1 2 d S T P . .
N002 N 0.60081(7) 0.27123(7) 0.34841(8) 0.01377(16) Uani 1 1 d . . . . .
N003 N 0.61836(8) 0.46705(8) 0.18326(8) 0.01647(17) Uani 1 1 d . . . . .
C004 C 0.71048(8) 0.28083(9) 0.34595(9) 0.01414(18) Uani 1 1 d . . . . .
C005 C 0.72528(9) 0.45009(9) 0.20312(9) 0.01565(19) Uani 1 1 d . . . . .
C006 C 0.55225(9) 0.18365(9) 0.42510(10) 0.0189(2) Uani 1 1 d . . . . .
H00A H 0.574121 0.194786 0.509068 0.028 Uiso 1 1 calc R U . . .
H00B H 0.577822 0.111949 0.397494 0.028 Uiso 1 1 calc R U . . .
H00C H 0.472914 0.186721 0.419111 0.028 Uiso 1 1 calc R U . . .
C007 C 0.76806(10) 0.36250(10) 0.27689(11) 0.0172(2) Uani 1 1 d . . . . .
C008 C 0.78118(9) 0.20237(10) 0.42096(10) 0.0197(2) Uani 1 1 d . . . . .
H00D H 0.763920 0.211235 0.506554 0.030 Uiso 1 1 calc R U . . .
H00E H 0.858033 0.219231 0.407572 0.030 Uiso 1 1 calc R U . . .
H00F H 0.766578 0.126708 0.396488 0.030 Uiso 1 1 calc R U . . .
C009 C 0.81031(10) 0.52724(10) 0.14601(11) 0.0213(2) Uani 1 1 d . . . . .
H00G H 0.800570 0.528424 0.058428 0.032 Uiso 1 1 calc R U . . .
H00H H 0.883454 0.500894 0.165210 0.032 Uiso 1 1 calc R U . . .
H00I H 0.800855 0.601345 0.178154 0.032 Uiso 1 1 calc R U . . .
C00A C 0.58592(11) 0.56558(10) 0.11180(12) 0.0249(2) Uani 1 1 d . . . . .
H00J H 0.614946 0.559443 0.029905 0.037 Uiso 1 1 calc R U . . .
H00K H 0.615025 0.631576 0.150208 0.037 Uiso 1 1 calc R U . . .
H00L H 0.506536 0.570253 0.108468 0.037 Uiso 1 1 calc R U . . .
H007 H 0.8467(14) 0.3617(12) 0.2827(15) 0.024(4) Uiso 1 1 d . . . . .
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
N002 Zn01 N002 108.62(5) 3_655 . ?
N003 Zn01 N002 95.98(4) 3_655 3_655 ?
N003 Zn01 N002 95.98(4) . . ?
N003 Zn01 N002 125.99(4) . 3_655 ?
N003 Zn01 N002 125.99(4) 3_655 . ?
N003 Zn01 N003 107.27(5) . 3_655 ?
C004 N002 Zn01 123.09(7) . . ?
C004 N002 C006 118.20(9) . . ?
C006 N002 Zn01 118.69(7) . . ?
C005 N003 Zn01 123.31(8) . . ?
C005 N003 C00A 118.05(9) . . ?
C00A N003 Zn01 118.62(7) . . ?
N002 C004 C007 124.02(10) . . ?
N002 C004 C008 119.90(9) . . ?
C007 C004 C008 116.07(10) . . ?
N003 C005 C007 124.10(10) . . ?
N003 C005 C009 120.01(10) . . ?
C007 C005 C009 115.89(10) . . ?
N002 C006 H00A 109.5 . . ?
N002 C006 H00B 109.5 . . ?
N002 C006 H00C 109.5 . . ?
H00A C006 H00B 109.5 . . ?
H00A C006 H00C 109.5 . . ?
H00B C006 H00C 109.5 . . ?
C004 C007 C005 129.24(11) . . ?
C004 C007 H007 116.6(10) . . ?
C005 C007 H007 114.1(10) . . ?
C004 C008 H00D 109.5 . . ?
C004 C008 H00E 109.5 . . ?
C004 C008 H00F 109.5 . . ?
H00D C008 H00E 109.5 . . ?
H00D C008 H00F 109.5 . . ?
H00E C008 H00F 109.5 . . ?
C005 C009 H00G 109.5 . . ?
C005 C009 H00H 109.5 . . ?
C005 C009 H00I 109.5 . . ?
H00G C009 H00H 109.5 . . ?
H00G C009 H00I 109.5 . . ?
H00H C009 H00I 109.5 . . ?
N003 C00A H00J 109.5 . . ?
N003 C00A H00K 109.5 . . ?
N003 C00A H00L 109.5 . . ?
H00J C00A H00K 109.5 . . ?
H00J C00A H00L 109.5 . . ?
H00K C00A H00L 109.5 . . ?
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
Zn01 N002 1.9948(9) . ?
Zn01 N002 1.9947(9) 3_655 ?
Zn01 N003 1.9892(9) 3_655 ?
Zn01 N003 1.9892(9) . ?
N002 C004 1.3283(13) . ?
N002 C006 1.4620(14) . ?
N003 C005 1.3235(14) . ?
N003 C00A 1.4654(14) . ?
C004 C007 1.4150(15) . ?
C004 C008 1.5082(14) . ?
C005 C007 1.4173(16) . ?
C005 C009 1.5135(15) . ?
C006 H00A 0.9600 . ?
C006 H00B 0.9600 . ?
C006 H00C 0.9600 . ?
C007 H007 0.950(17) . ?
C008 H00D 0.9600 . ?
C008 H00E 0.9600 . ?
C008 H00F 0.9600 . ?
C009 H00G 0.9600 . ?
C009 H00H 0.9600 . ?
C009 H00I 0.9600 . ?
C00A H00J 0.9600 . ?
C00A H00K 0.9600 . ?
C00A H00L 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn01 N002 C004 C007 2.00(14) . . . . ?
Zn01 N002 C004 C008 -178.65(7) . . . . ?
Zn01 N003 C005 C007 -2.07(15) . . . . ?
Zn01 N003 C005 C009 178.29(7) . . . . ?
N002 C004 C007 C005 2.66(18) . . . . ?
N003 C005 C007 C004 -2.63(19) . . . . ?
C006 N002 C004 C007 -179.27(10) . . . . ?
C006 N002 C004 C008 0.08(14) . . . . ?
C008 C004 C007 C005 -176.71(11) . . . . ?
C009 C005 C007 C004 177.02(10) . . . . ?
C00A N003 C005 C007 175.88(10) . . . . ?
C00A N003 C005 C009 -3.76(15) . . . . ?
