#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/24/7052419.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_7052419
loop_
_publ_author_name
'Cole, Marcus L.'
'Junk, Peter C.'
_publ_section_title
;
 N,N?-Bis(2,6-diisopropylphenyl)formamidinate complexes of the heavy
 alkaline earths
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              135
_journal_paper_doi               10.1039/b411494a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety         'C31 H36 F4 N2'
_chemical_formula_sum            'C31 H36 F4 N2'
_chemical_formula_weight         512.62
_chemical_melting_point          451
_chemical_name_common            DippN(4-HC6F4)C(H)NDipp
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.256(3)
_cell_angle_beta                 91.904(2)
_cell_angle_gamma                106.1040(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4525(4)
_cell_length_b                   11.4180(5)
_cell_length_c                   14.3724(7)
_cell_measurement_temperature    123(2)
_cell_volume                     1383.70(11)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20737
_diffrn_reflns_theta_full        27.79
_diffrn_reflns_theta_max         27.79
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9866
_exptl_absorpt_correction_T_min  0.9734
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN program'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0490
_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)+(0.1055P)²+0.1303P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1659
_reflns_number_gt                4552
_reflns_number_total             6442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b411494a.txt
_cod_data_source_block           Compound4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7052419
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
F1 F 0.25058(10) 0.02346(9) 0.10983(7) 0.0267(2) Uani 1 1 d . . .
F2 F 0.30495(12) -0.16395(10) -0.04086(7) 0.0323(3) Uani 1 1 d . . .
F3 F 0.75015(11) -0.11064(10) 0.14956(8) 0.0320(3) Uani 1 1 d . . .
F4 F 0.70078(10) 0.07974(9) 0.30021(7) 0.0254(2) Uani 1 1 d . . .
N1 N 0.44953(14) 0.16415(12) 0.29207(9) 0.0188(3) Uani 1 1 d . . .
N2 N 0.43495(14) 0.28872(12) 0.19527(10) 0.0201(3) Uani 1 1 d . . .
C1 C 0.44579(17) 0.15764(15) 0.39144(12) 0.0200(3) Uani 1 1 d . . .
C2 C 0.31926(18) 0.07315(16) 0.40881(12) 0.0233(3) Uani 1 1 d . . .
C3 C 0.31718(19) 0.06636(17) 0.50327(13) 0.0287(4) Uani 1 1 d . . .
H3 H 0.2344 0.0072 0.5158 0.034 Uiso 1 1 calc R . .
C4 C 0.4346(2) 0.14501(18) 0.57975(14) 0.0305(4) Uani 1 1 d . . .
H4 H 0.4321 0.1389 0.6440 0.037 Uiso 1 1 calc R . .
C5 C 0.5544(2) 0.23169(17) 0.56258(13) 0.0272(4) Uani 1 1 d . . .
H5 H 0.6318 0.2879 0.6164 0.033 Uiso 1 1 calc R . .
C6 C 0.56535(18) 0.23924(15) 0.46810(12) 0.0217(3) Uani 1 1 d . . .
C7 C 0.18103(19) -0.00158(18) 0.33059(14) 0.0300(4) Uani 1 1 d . . .
H7 H 0.2080 0.0038 0.2652 0.036 Uiso 1 1 calc R . .
C8 C 0.1227(3) -0.1450(2) 0.3161(2) 0.0752(10) Uani 1 1 d . . .
H8A H 0.0891 -0.1530 0.3781 0.113 Uiso 1 1 calc R . .
H8B H 0.2020 -0.1854 0.2995 0.113 Uiso 1 1 calc R . .
H8C H 0.0390 -0.1896 0.2615 0.113 Uiso 1 1 calc R . .
C9 C 0.0609(3) 0.0634(3) 0.3589(2) 0.0637(8) Uani 1 1 d . . .
H9A H 0.0255 0.0518 0.4194 0.096 Uiso 1 1 calc R . .
H9B H -0.0222 0.0233 0.3039 0.096 Uiso 1 1 calc R . .
H9C H 0.1017 0.1573 0.3718 0.096 Uiso 1 1 calc R . .
C10 C 0.70217(18) 0.33632(15) 0.45427(12) 0.0220(3) Uani 1 1 d . . .
H10 H 0.6990 0.3207 0.3812 0.026 Uiso 1 1 calc R . .
C11 C 0.84733(19) 0.32008(17) 0.49116(14) 0.0288(4) Uani 1 1 d . . .
H11A H 0.8587 0.3465 0.5642 0.043 Uiso 1 1 calc R . .
H11B H 0.9318 0.3754 0.4724 0.043 Uiso 1 1 calc R . .
H11C H 0.8441 0.2280 0.4604 0.043 Uiso 1 1 calc R . .
C12 C 0.7023(2) 0.47804(16) 0.51058(14) 0.0292(4) Uani 1 1 d . . .
H12A H 0.6135 0.4911 0.4840 0.044 Uiso 1 1 calc R . .
H12B H 0.7915 0.5393 0.5016 0.044 Uiso 1 1 calc R . .
H12C H 0.7018 0.4940 0.5821 0.044 Uiso 1 1 calc R . .
C13 C 0.40115(18) 0.40004(15) 0.18816(11) 0.0207(3) Uani 1 1 d . . .
C14 C 0.51847(19) 0.50163(16) 0.18015(12) 0.0242(4) Uani 1 1 d . . .
C15 C 0.4858(2) 0.60781(17) 0.16831(13) 0.0289(4) Uani 1 1 d . . .
H15 H 0.5641 0.6772 0.1629 0.035 Uiso 1 1 calc R . .
C16 C 0.3425(2) 0.61424(17) 0.16421(14) 0.0317(4) Uani 1 1 d . . .
H16 H 0.3227 0.6881 0.1571 0.038 Uiso 1 1 calc R . .
C17 C 0.2272(2) 0.51216(17) 0.17045(13) 0.0283(4) Uani 1 1 d . . .
H17 H 0.1286 0.5170 0.1673 0.034 Uiso 1 1 calc R . .
C18 C 0.25287(18) 0.40246(15) 0.18122(12) 0.0228(3) Uani 1 1 d . . .
C19 C 0.6781(2) 0.49894(17) 0.18846(14) 0.0307(4) Uani 1 1 d . . .
H19 H 0.6749 0.4062 0.1751 0.037 Uiso 1 1 calc R . .
C20 C 0.7643(3) 0.5422(3) 0.11288(18) 0.0537(6) Uani 1 1 d . . .
H20A H 0.7092 0.4906 0.0454 0.081 Uiso 1 1 calc R . .
H20B H 0.8619 0.5287 0.1163 0.081 Uiso 1 1 calc R . .
H20C H 0.7774 0.6355 0.1280 0.081 Uiso 1 1 calc R . .
C21 C 0.7577(3) 0.5813(3) 0.29379(17) 0.0504(6) Uani 1 1 d . . .
H21A H 0.8584 0.5743 0.2992 0.076 Uiso 1 1 calc R . .
H21B H 0.7028 0.5498 0.3415 0.076 Uiso 1 1 calc R . .
H21C H 0.7635 0.6732 0.3089 0.076 Uiso 1 1 calc R . .
C22 C 0.12168(19) 0.28625(16) 0.17634(13) 0.0276(4) Uani 1 1 d . . .
H22 H 0.1598 0.2333 0.2079 0.033 Uiso 1 1 calc R . .
C23 C 0.0608(2) 0.1991(2) 0.06677(15) 0.0405(5) Uani 1 1 d . . .
H23A H 0.0205 0.2478 0.0342 0.061 Uiso 1 1 calc R . .
H23B H -0.0182 0.1207 0.0636 0.061 Uiso 1 1 calc R . .
H23C H 0.1412 0.1729 0.0323 0.061 Uiso 1 1 calc R . .
C24 C -0.0026(2) 0.3253(2) 0.23230(15) 0.0375(5) Uani 1 1 d . . .
H24A H 0.0387 0.3839 0.3016 0.056 Uiso 1 1 calc R . .
H24B H -0.0781 0.2464 0.2320 0.056 Uiso 1 1 calc R . .
H24C H -0.0483 0.3706 0.1992 0.056 Uiso 1 1 calc R . .
C25 C 0.42554(16) 0.27053(14) 0.27696(11) 0.0186(3) Uani 1 1 d . . .
H25 H 0.4005 0.3338 0.3312 0.022 Uiso 1 1 calc R . .
C26 C 0.47481(17) 0.06085(14) 0.21137(11) 0.0182(3) Uani 1 1 d . . .
C27 C 0.37608(17) -0.00601(14) 0.12183(12) 0.0204(3) Uani 1 1 d . . .
C28 C 0.40399(19) -0.10510(15) 0.04352(12) 0.0232(3) Uani 1 1 d . . .
C29 C 0.52850(19) -0.14329(15) 0.04996(12) 0.0250(4) Uani 1 1 d . . .
H29 H 0.5469 -0.2112 -0.0041 0.030 Uiso 1 1 calc R . .
C30 C 0.62527(18) -0.07875(15) 0.13827(13) 0.0230(3) Uani 1 1 d . . .
C31 C 0.59937(17) 0.02010(14) 0.21714(12) 0.0191(3) Uani 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'
F F 0.0171 0.0103 '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
C25 N1 C26 120.56(13) . . ?
C25 N1 C1 119.19(12) . . ?
C26 N1 C1 120.24(12) . . ?
C25 N2 C13 118.26(13) . . ?
C2 C1 C6 121.83(15) . . ?
C2 C1 N1 118.54(13) . . ?
C6 C1 N1 119.58(14) . . ?
C3 C2 C1 118.22(15) . . ?
C3 C2 C7 119.44(15) . . ?
C1 C2 C7 122.15(15) . . ?
C4 C3 C2 120.85(16) . . ?
C5 C4 C3 120.04(16) . . ?
C4 C5 C6 121.65(16) . . ?
C5 C6 C1 117.29(15) . . ?
C5 C6 C10 118.78(14) . . ?
C1 C6 C10 123.91(14) . . ?
C8 C7 C9 110.2(2) . . ?
C8 C7 C2 112.99(16) . . ?
C9 C7 C2 109.69(16) . . ?
C6 C10 C11 112.07(13) . . ?
C6 C10 C12 110.49(13) . . ?
C11 C10 C12 108.96(13) . . ?
C14 C13 C18 121.26(14) . . ?
C14 C13 N2 117.84(14) . . ?
C18 C13 N2 120.70(14) . . ?
C15 C14 C13 118.41(15) . . ?
C15 C14 C19 120.54(15) . . ?
C13 C14 C19 121.00(14) . . ?
C16 C15 C14 121.40(17) . . ?
C15 C16 C17 119.64(15) . . ?
C16 C17 C18 121.55(16) . . ?
C17 C18 C13 117.69(16) . . ?
C17 C18 C22 119.76(15) . . ?
C13 C18 C22 122.35(14) . . ?
C21 C19 C20 110.48(18) . . ?
C21 C19 C14 110.31(16) . . ?
C20 C19 C14 113.11(16) . . ?
C18 C22 C24 113.86(14) . . ?
C18 C22 C23 109.48(16) . . ?
C24 C22 C23 110.38(15) . . ?
N2 C25 N1 123.85(13) . . ?
C31 C26 C27 116.05(13) . . ?
C31 C26 N1 121.81(13) . . ?
C27 C26 N1 122.14(13) . . ?
F1 C27 C28 118.12(13) . . ?
F1 C27 C26 120.67(13) . . ?
C28 C27 C26 121.20(14) . . ?
F2 C28 C29 120.05(14) . . ?
F2 C28 C27 117.90(14) . . ?
C29 C28 C27 122.05(15) . . ?
C28 C29 C30 117.00(14) . . ?
F3 C30 C29 120.18(14) . . ?
F3 C30 C31 118.00(14) . . ?
C29 C30 C31 121.82(15) . . ?
F4 C31 C30 118.08(13) . . ?
F4 C31 C26 120.03(13) . . ?
C30 C31 C26 121.86(14) . . ?
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
F1 C27 1.3410(17) . ?
F2 C28 1.3454(18) . ?
F3 C30 1.3486(18) . ?
F4 C31 1.3442(17) . ?
N1 C25 1.3806(19) . ?
N1 C26 1.4216(19) . ?
N1 C1 1.457(2) . ?
N2 C25 1.263(2) . ?
N2 C13 1.4287(19) . ?
C1 C2 1.404(2) . ?
C1 C6 1.408(2) . ?
C2 C3 1.387(2) . ?
C2 C7 1.523(2) . ?
C3 C4 1.389(2) . ?
C4 C5 1.375(3) . ?
C5 C6 1.395(2) . ?
C6 C10 1.522(2) . ?
C7 C8 1.512(3) . ?
C7 C9 1.515(3) . ?
C10 C11 1.536(2) . ?
C10 C12 1.538(2) . ?
C13 C14 1.406(2) . ?
C13 C18 1.410(2) . ?
C14 C15 1.393(2) . ?
C14 C19 1.519(2) . ?
C15 C16 1.377(3) . ?
C16 C17 1.389(3) . ?
C17 C18 1.397(2) . ?
C18 C22 1.523(2) . ?
C19 C21 1.513(3) . ?
C19 C20 1.515(3) . ?
C22 C24 1.527(2) . ?
C22 C23 1.529(3) . ?
C26 C31 1.391(2) . ?
C26 C27 1.398(2) . ?
C27 C28 1.386(2) . ?
C28 C29 1.375(2) . ?
C29 C30 1.375(2) . ?
C30 C31 1.380(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21189302
