#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:58:44 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289510 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/47/7714706.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_7714706
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_sum            'C36 H72 Ca Cl2 N12 O14'
_chemical_formula_weight         1008.04
_chemical_name_systematic
; 
Hexakis(dimethylpropyleneurea)calcium(II)perchlorate
;
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2023-09-26 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   13.083(3)
_cell_length_b                   13.083(3)
_cell_length_c                   8.553(3)
_cell_measurement_reflns_used    1270
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.80
_cell_volume                     1267.8(6)
_computing_cell_refinement       'Bruker SMART and SAINT (1998)'
_computing_data_collection       'Bruker SMART (1998)'
_computing_data_reduction        'Bruker SAINT (1998)'
_computing_molecular_graphics    'Bruker SHELXTL (1998)'
_computing_publication_material  'Bruker SHELXTL (1998)'
_computing_structure_refinement  'Bruker SHELXTL (1998)'
_computing_structure_solution    'Bruker SHELXTL (1998)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'Omega 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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9888
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%
;
Neglible as determined from a repetition of the first
50 frames at the end of the experiment
;
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.8896
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                1270
_reflns_number_total             1914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt03193d2.cif
_cod_data_source_block           ca_dmpu6_clo4_2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Hexagonal' was changed to
'hexagonal' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7714702--7714710.cif.
;
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7714706
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.0000 0.0000 0.0000 0.0371(3) Uani 1 6 d S . .
O1 O 0.10765(11) 0.16565(10) 0.15653(15) 0.0527(4) Uani 1 1 d . . .
N1 N 0.26955(15) 0.25712(15) 0.3090(2) 0.0609(5) Uani 1 1 d . . .
N2 N 0.20174(16) 0.36425(14) 0.1741(2) 0.0628(5) Uani 1 1 d . . .
C1 C 0.18980(15) 0.25856(15) 0.21082(19) 0.0452(4) Uani 1 1 d . . .
C2 C 0.3688(2) 0.3628(2) 0.3746(3) 0.0786(7) Uani 1 1 d . . .
H2A H 0.4369 0.3520 0.3806 0.094 Uiso 1 1 calc R . .
H2B H 0.3494 0.3748 0.4800 0.094 Uiso 1 1 calc R . .
C3 C 0.3986(3) 0.4670(3) 0.2806(4) 0.1110(11) Uani 1 1 d . . .
H4A H 0.4510 0.5370 0.3403 0.133 Uiso 1 1 calc R . .
H4B H 0.4409 0.4659 0.1880 0.133 Uiso 1 1 calc R . .
C4 C 0.2966(3) 0.4750(2) 0.2327(4) 0.1006(10) Uani 1 1 d . . .
H3A H 0.2681 0.5000 0.3212 0.121 Uiso 1 1 calc R . .
H3B H 0.3200 0.5346 0.1519 0.121 Uiso 1 1 calc R . .
C5 C 0.2562(3) 0.1450(3) 0.3571(4) 0.0975(9) Uani 1 1 d . . .
H5A H 0.2593 0.1425 0.4691 0.146 Uiso 1 1 calc R . .
H5B H 0.3187 0.1361 0.3131 0.146 Uiso 1 1 calc R . .
H5C H 0.1815 0.0821 0.3211 0.146 Uiso 1 1 calc R . .
C6 C 0.1162(3) 0.3689(2) 0.0726(4) 0.1026(11) Uani 1 1 d . . .
H6A H 0.1356 0.4495 0.0594 0.154 Uiso 1 1 calc R . .
H6B H 0.0391 0.3245 0.1182 0.154 Uiso 1 1 calc R . .
H6C H 0.1169 0.3359 -0.0273 0.154 Uiso 1 1 calc R . .
Cl1 Cl -0.3333 0.3333 0.26775(18) 0.0893(4) Uani 1 3 d S . .
O3A O -0.3342(8) 0.4325(9) 0.3225(18) 0.184(9) Uani 0.49(2) 1 d P . .
O3B O -0.3500(10) 0.4182(10) 0.2007(16) 0.184(7) Uani 0.51(2) 1 d P . .
O4A O -0.3333 0.3333 0.1166(18) 0.229(12) Uani 0.49(2) 3 d SP . .
O4B O -0.3333 0.3333 0.4177(13) 0.240(12) Uani 0.51(2) 3 d SP . .
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'
Cl Cl 0.1484 0.1585 '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'
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 180.00(8) 4 . ?
O1 Ca1 O1 90.23(5) 4 6 ?
O1 Ca1 O1 89.77(5) . 6 ?
O1 Ca1 O1 89.77(5) 4 2 ?
O1 Ca1 O1 90.23(5) . 2 ?
O1 Ca1 O1 89.77(5) 6 2 ?
O1 Ca1 O1 90.23(5) 4 5 ?
O1 Ca1 O1 89.77(5) . 5 ?
O1 Ca1 O1 90.23(5) 6 5 ?
O1 Ca1 O1 180.0 2 5 ?
O1 Ca1 O1 89.77(5) 4 3 ?
O1 Ca1 O1 90.23(5) . 3 ?
O1 Ca1 O1 180.00(7) 6 3 ?
O1 Ca1 O1 90.23(5) 2 3 ?
O1 Ca1 O1 89.77(5) 5 3 ?
C1 O1 Ca1 161.97(12) . . ?
C1 N1 C5 119.30(18) . . ?
C1 N1 C2 123.84(18) . . ?
C5 N1 C2 116.84(19) . . ?
C1 N2 C6 119.31(17) . . ?
C1 N2 C4 123.21(18) . . ?
C6 N2 C4 117.48(19) . . ?
O1 C1 N1 121.12(17) . . ?
O1 C1 N2 121.08(17) . . ?
N1 C1 N2 117.79(16) . . ?
N1 C2 C3 111.7(2) . . ?
C4 C3 C2 113.5(3) . . ?
N2 C4 C3 112.7(2) . . ?
O4B Cl1 O4A 180.000(5) . . ?
O4B Cl1 O3B 114.9(7) . 3_455 ?
O4A Cl1 O3B 65.1(7) . 3_455 ?
O4B Cl1 O3B 114.9(7) . 2_565 ?
O4A Cl1 O3B 65.1(7) . 2_565 ?
O3B Cl1 O3B 103.5(8) 3_455 2_565 ?
O4B Cl1 O3B 114.9(7) . . ?
O4A Cl1 O3B 65.1(7) . . ?
O3B Cl1 O3B 103.5(8) 3_455 . ?
O3B Cl1 O3B 103.5(8) 2_565 . ?
O4B Cl1 O3A 70.2(7) . 3_455 ?
O4A Cl1 O3A 109.8(7) . 3_455 ?
O3B Cl1 O3A 45.4(5) 3_455 3_455 ?
O3B Cl1 O3A 117.2(8) 2_565 3_455 ?
O3B Cl1 O3A 132.2(7) . 3_455 ?
O4B Cl1 O3A 70.2(7) . 2_565 ?
O4A Cl1 O3A 109.8(7) . 2_565 ?
O3B Cl1 O3A 132.2(7) 3_455 2_565 ?
O3B Cl1 O3A 45.4(5) 2_565 2_565 ?
O3B Cl1 O3A 117.2(8) . 2_565 ?
O3A Cl1 O3A 109.2(7) 3_455 2_565 ?
O4B Cl1 O3A 70.2(7) . . ?
O4A Cl1 O3A 109.8(7) . . ?
O3B Cl1 O3A 117.2(8) 3_455 . ?
O3B Cl1 O3A 132.2(7) 2_565 . ?
O3B Cl1 O3A 45.4(5) . . ?
O3A Cl1 O3A 109.2(7) 3_455 . ?
O3A Cl1 O3A 109.2(7) 2_565 . ?
O3B O3A Cl1 66.1(6) . . ?
O3B O3A O4B 117.1(11) . . ?
Cl1 O3A O4B 51.8(6) . . ?
O3A O3B Cl1 68.5(8) . . ?
O3A O3B O4A 122.6(13) . . ?
Cl1 O3B O4A 55.2(7) . . ?
Cl1 O4A O3B 59.8(7) . 3_455 ?
Cl1 O4A O3B 59.8(7) . 2_565 ?
O3B O4A O3B 96.9(9) 3_455 2_565 ?
Cl1 O4A O3B 59.8(7) . . ?
O3B O4A O3B 96.9(9) 3_455 . ?
O3B O4A O3B 96.9(9) 2_565 . ?
Cl1 O4B O3A 58.0(5) . 3_455 ?
Cl1 O4B O3A 58.0(5) . 2_565 ?
O3A O4B O3A 94.5(7) 3_455 2_565 ?
Cl1 O4B O3A 58.0(5) . . ?
O3A O4B O3A 94.5(7) 3_455 . ?
O3A O4B O3A 94.5(7) 2_565 . ?
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 2.3282(12) 4 ?
Ca1 O1 2.3282(12) . ?
Ca1 O1 2.3282(12) 6 ?
Ca1 O1 2.3282(12) 2 ?
Ca1 O1 2.3282(12) 5 ?
Ca1 O1 2.3282(12) 3 ?
O1 C1 1.242(2) . ?
N1 C1 1.347(2) . ?
N1 C5 1.447(3) . ?
N1 C2 1.455(3) . ?
N2 C1 1.349(2) . ?
N2 C6 1.441(3) . ?
N2 C4 1.446(3) . ?
C2 C3 1.459(4) . ?
C3 C4 1.448(4) . ?
Cl1 O4B 1.282(11) . ?
Cl1 O4A 1.293(15) . ?
Cl1 O3B 1.361(8) 3_455 ?
Cl1 O3B 1.361(8) 2_565 ?
Cl1 O3B 1.361(8) . ?
Cl1 O3A 1.385(7) 3_455 ?
Cl1 O3A 1.385(7) 2_565 ?
Cl1 O3A 1.385(7) . ?
O3A O3B 1.061(11) . ?
O3A O4B 1.536(16) . ?
O3B O4A 1.429(16) . ?
O4A O3B 1.429(16) 3_455 ?
O4A O3B 1.429(16) 2_565 ?
O4B O3A 1.536(16) 3_455 ?
O4B O3A 1.536(16) 2_565 ?
