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#$Date: 2024-02-04 13:58:44 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289510 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/47/7714704.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_7714704
loop_
_publ_author_name
'Lundberg, Daniel'
'Lindqvist-Reis, Patric'
'Łyczko, Krzysztof'
'Eriksson, Lars'
'Persson, Ingmar'
_publ_section_title
;
 Coordination chemistry effects of the space-demanding solvent molecule
 N,N'-dimethylpropyleneurea.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1817
_journal_page_last               1832
_journal_paper_doi               10.1039/d3dt03193d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H72 Ca N12 O6, 2(I)'
_chemical_formula_sum            'C36 H72 Ca I2 N12 O6'
_chemical_formula_weight         1062.93
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-08 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   12.9549(18)
_cell_length_b                   12.9549(18)
_cell_length_c                   8.5602(12)
_cell_measurement_reflns_used    2024
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.5
_cell_measurement_theta_min      3.70
_cell_volume                     1244.2(3)
_computing_cell_refinement       'APEX3 (Bruker, 2020)'
_computing_data_collection       'APEX3 (Bruker, 2020)'
_computing_data_reduction        'APEX3 (Bruker, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'ω scans and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7894
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.536
_diffrn_reflns_theta_max         23.536
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'Incotec 1MyS'
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0043(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0494
_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)+(0.0545P)²+1.7945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1100
_reflns_number_total             1246
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03193d2.cif
_cod_data_source_block           Ca_dmpu6_I2
_cod_depositor_comments
'Adding full bibliography for 7714702--7714710.cif.'
_cod_original_cell_volume        1244.2(4)
_cod_database_code               7714704
_shelx_shelxl_version_number     2018/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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
I1 I 0.666667 0.333333 0.21996(15) 0.1436(6) Uani 1 3 d S T P . .
Ca1 Ca 1.000000 0.000000 0.500000 0.0371(4) Uani 1 6 d S T P . .
O1 O 0.8337(2) -0.0562(2) 0.3443(3) 0.0534(7) Uani 1 1 d . . . . .
C1 C 0.7398(3) -0.0666(3) 0.2897(4) 0.0461(9) Uani 1 1 d . . . . .
N11 N 0.6336(3) -0.1591(3) 0.3287(4) 0.0658(10) Uani 1 1 d . . . . .
N12 N 0.7420(3) 0.0139(3) 0.1908(4) 0.0622(9) Uani 1 1 d . . . . .
C11 C 0.6286(5) -0.2484(5) 0.4347(8) 0.114(2) Uani 1 1 d . . . . .
H11A H 0.658688 -0.293851 0.383223 0.170 Uiso 1 1 calc R U . . .
H11B H 0.547523 -0.300537 0.465897 0.170 Uiso 1 1 calc R U . . .
H11C H 0.676268 -0.210162 0.525205 0.170 Uiso 1 1 calc R U . . .
C12 C 0.8549(5) 0.1130(6) 0.1410(7) 0.107(2) Uani 1 1 d . . . . .
H12A H 0.917432 0.095851 0.162890 0.160 Uiso 1 1 calc R U . . .
H12B H 0.869824 0.183669 0.196181 0.160 Uiso 1 1 calc R U . . .
H12C H 0.852292 0.125242 0.030767 0.160 Uiso 1 1 calc R U . . .
C13 C 0.5215(4) -0.1750(6) 0.2718(8) 0.103(2) Uani 1 1 d . . . . .
H13A H 0.494065 -0.231224 0.185779 0.124 Uiso 1 1 calc R U . . .
H13B H 0.462590 -0.208599 0.354541 0.124 Uiso 1 1 calc R U . . .
C14 C 0.5308(5) -0.0658(7) 0.2204(10) 0.121(2) Uani 1 1 d . . . . .
H14A H 0.532916 -0.020036 0.311249 0.145 Uiso 1 1 calc R U . . .
H14B H 0.459978 -0.083934 0.160924 0.145 Uiso 1 1 calc R U . . .
C15 C 0.6353(5) 0.0073(5) 0.1246(6) 0.0827(15) Uani 1 1 d . . . . .
H15A H 0.646683 0.087045 0.116263 0.099 Uiso 1 1 calc R U . . .
H15B H 0.622379 -0.026141 0.020272 0.099 Uiso 1 1 calc R U . . .
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
O1 Ca1 O1 90.27(9) 4_756 5_666 ?
O1 Ca1 O1 89.73(9) 4_756 2_645 ?
O1 Ca1 O1 180.0 5_666 2_645 ?
O1 Ca1 O1 90.27(9) 4_756 6_546 ?
O1 Ca1 O1 90.27(9) 5_666 6_546 ?
O1 Ca1 O1 89.73(9) 2_645 6_546 ?
O1 Ca1 O1 89.73(9) 4_756 3_765 ?
O1 Ca1 O1 89.73(9) 5_666 3_765 ?
O1 Ca1 O1 90.27(9) 2_645 3_765 ?
O1 Ca1 O1 180.00(11) 6_546 3_765 ?
O1 Ca1 O1 180.0 4_756 . ?
O1 Ca1 O1 89.72(9) 5_666 . ?
O1 Ca1 O1 90.28(9) 2_645 . ?
O1 Ca1 O1 89.72(9) 6_546 . ?
O1 Ca1 O1 90.28(9) 3_765 . ?
C1 O1 Ca1 162.4(2) . . ?
O1 C1 N12 121.1(3) . . ?
O1 C1 N11 121.0(3) . . ?
N12 C1 N11 117.9(3) . . ?
C1 N11 C13 123.6(4) . . ?
C1 N11 C11 119.2(3) . . ?
C13 N11 C11 117.2(4) . . ?
C1 N12 C12 119.9(4) . . ?
C1 N12 C15 123.6(4) . . ?
C12 N12 C15 116.5(4) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N11 112.4(5) . . ?
C14 C13 H13A 109.1 . . ?
N11 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
N11 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 C15 114.1(5) . . ?
C13 C14 H14A 108.7 . . ?
C15 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
C15 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 N12 111.4(4) . . ?
C14 C15 H15A 109.3 . . ?
N12 C15 H15A 109.3 . . ?
C14 C15 H15B 109.3 . . ?
N12 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
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
Ca1 O1 2.319(2) 4_756 ?
Ca1 O1 2.319(2) 5_666 ?
Ca1 O1 2.319(2) 2_645 ?
Ca1 O1 2.319(2) 6_546 ?
Ca1 O1 2.319(2) 3_765 ?
Ca1 O1 2.319(2) . ?
O1 C1 1.246(4) . ?
C1 N12 1.333(5) . ?
C1 N11 1.338(5) . ?
N11 C13 1.446(5) . ?
N11 C11 1.446(6) . ?
N12 C12 1.446(6) . ?
N12 C15 1.456(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.428(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.456(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
