#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:07:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179776 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007241.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_7007241
loop_
_publ_author_name
'Cole, Marcus L.'
'Deacon, Glen B.'
'Forsyth, Craig M.'
'Konstas, Kristina'
'Junk, Peter C.'
_publ_section_title
;
 Synthesis and structural characterisation of heavy alkaline earth
 N,N'-bis(aryl)formamidinate complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3360
_journal_page_last               3367
_journal_paper_doi               10.1039/b602210c
_journal_year                    2006
_chemical_compound_source        THF
_chemical_formula_moiety         'C38 H46 Ca N4 O2'
_chemical_formula_sum            'C38 H46 Ca N4 O2'
_chemical_formula_weight         630.87
_chemical_melting_point          441(2)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.930(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2249(3)
_cell_length_b                   16.7282(9)
_cell_length_c                   19.6462(10)
_cell_measurement_temperature    123(2)
_cell_volume                     3547.3(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.1092
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23008
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.9894
_exptl_absorpt_correction_T_min  0.9385
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.777
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.777
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1373P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1810
_reflns_number_gt                4683
_reflns_number_total             8358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602210c.txt
_cod_data_source_block           COMPOUND_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '439-443' was changed to '441(2)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7007241
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.28026(4) 0.01301(3) 0.77356(2) 0.02077(15) Uani 1 1 d . . .
O1 O 0.20721(15) 0.05329(10) 0.87038(8) 0.0281(4) Uani 1 1 d . . .
O2 O 0.35667(15) -0.04064(11) 0.68216(9) 0.0299(4) Uani 1 1 d . . .
N1 N 0.25600(16) 0.14304(12) 0.71807(10) 0.0228(5) Uani 1 1 d . . .
N2 N 0.43788(16) 0.11759(12) 0.80313(9) 0.0218(5) Uani 1 1 d . . .
N3 N 0.09817(16) -0.07132(12) 0.73704(10) 0.0226(5) Uani 1 1 d . . .
N4 N 0.27408(16) -0.12470(12) 0.81098(10) 0.0214(4) Uani 1 1 d . . .
C1 C 0.17839(19) 0.20060(15) 0.67591(12) 0.0206(5) Uani 1 1 d . . .
C2 C 0.0968(2) 0.17607(16) 0.61056(12) 0.0239(5) Uani 1 1 d . . .
C3 C 0.0210(2) 0.23347(17) 0.56922(13) 0.0277(6) Uani 1 1 d . . .
H3 H -0.0336 0.2178 0.5251 0.033 Uiso 1 1 calc R . .
C4 C 0.0219(2) 0.31249(17) 0.58974(13) 0.0300(6) Uani 1 1 d . . .
H4 H -0.0304 0.3503 0.5597 0.036 Uiso 1 1 calc R . .
C5 C 0.0993(2) 0.33629(17) 0.65426(13) 0.0305(6) Uani 1 1 d . . .
H5 H 0.1004 0.3904 0.6691 0.037 Uiso 1 1 calc R . .
C6 C 0.1757(2) 0.27986(16) 0.69723(13) 0.0257(6) Uani 1 1 d . . .
H6 H 0.2272 0.2958 0.7421 0.031 Uiso 1 1 calc R . .
C7 C 0.0940(2) 0.09092(17) 0.58617(13) 0.0344(7) Uani 1 1 d . . .
H7A H 0.0333 0.0855 0.5399 0.052 Uiso 1 1 calc R . .
H7B H 0.0706 0.0560 0.6204 0.052 Uiso 1 1 calc R . .
H7C H 0.1762 0.0757 0.5823 0.052 Uiso 1 1 calc R . .
C8 C 0.56293(19) 0.13904(14) 0.83314(12) 0.0200(5) Uani 1 1 d . . .
C9 C 0.6102(2) 0.13775(16) 0.90740(12) 0.0233(5) Uani 1 1 d . . .
C10 C 0.7340(2) 0.15891(16) 0.93692(13) 0.0272(6) Uani 1 1 d . . .
H10 H 0.7663 0.1593 0.9870 0.033 Uiso 1 1 calc R . .
C11 C 0.8109(2) 0.17933(15) 0.89553(13) 0.0252(6) Uani 1 1 d . . .
H11 H 0.8951 0.1926 0.9170 0.030 Uiso 1 1 calc R . .
C12 C 0.7644(2) 0.18031(15) 0.82269(13) 0.0247(6) Uani 1 1 d . . .
H12 H 0.8166 0.1945 0.7938 0.030 Uiso 1 1 calc R . .
C13 C 0.6409(2) 0.16041(15) 0.79177(12) 0.0230(5) Uani 1 1 d . . .
H13 H 0.6093 0.1614 0.7417 0.028 Uiso 1 1 calc R . .
C14 C 0.5287(2) 0.1173(2) 0.95381(13) 0.0412(8) Uani 1 1 d . . .
H14A H 0.5787 0.1151 1.0033 0.062 Uiso 1 1 calc R . .
H14B H 0.4899 0.0651 0.9399 0.062 Uiso 1 1 calc R . .
H14C H 0.4644 0.1582 0.9486 0.062 Uiso 1 1 calc R . .
C15 C 0.3695(2) 0.16525(14) 0.75447(12) 0.0205(5) Uani 1 1 d . . .
H15 H 0.4013 0.2156 0.7453 0.025 Uiso 1 1 calc R . .
C16 C -0.0159(2) -0.08383(15) 0.68614(12) 0.0212(5) Uani 1 1 d . . .
C17 C -0.1097(2) -0.02605(16) 0.68055(13) 0.0261(6) Uani 1 1 d . . .
C18 C -0.2229(2) -0.03804(18) 0.63054(14) 0.0361(7) Uani 1 1 d . . .
H18 H -0.2875 -0.0004 0.6272 0.043 Uiso 1 1 calc R . .
C19 C -0.2440(2) -0.10336(19) 0.58544(15) 0.0411(7) Uani 1 1 d . . .
H19 H -0.3227 -0.1105 0.5522 0.049 Uiso 1 1 calc R . .
C20 C -0.1504(2) -0.15811(17) 0.58898(14) 0.0362(7) Uani 1 1 d . . .
H20 H -0.1631 -0.2020 0.5571 0.043 Uiso 1 1 calc R . .
C21 C -0.0375(2) -0.14849(16) 0.63959(13) 0.0280(6) Uani 1 1 d . . .
H21 H 0.0263 -0.1867 0.6425 0.034 Uiso 1 1 calc R . .
C22 C -0.0884(2) 0.04592(18) 0.72775(15) 0.0379(7) Uani 1 1 d . . .
H22A H -0.1650 0.0772 0.7187 0.057 Uiso 1 1 calc R . .
H22B H -0.0228 0.0789 0.7181 0.057 Uiso 1 1 calc R . .
H22C H -0.0635 0.0287 0.7773 0.057 Uiso 1 1 calc R . .
C23 C 0.3349(2) -0.19066(15) 0.84916(12) 0.0218(5) Uani 1 1 d . . .
C24 C 0.4657(2) -0.19232(16) 0.86662(12) 0.0268(6) Uani 1 1 d . . .
C25 C 0.5278(2) -0.25848(19) 0.90323(13) 0.0353(7) Uani 1 1 d . . .
H25 H 0.6155 -0.2609 0.9139 0.042 Uiso 1 1 calc R . .
C26 C 0.4644(3) -0.32059(18) 0.92434(14) 0.0398(7) Uani 1 1 d . . .
H26 H 0.5085 -0.3650 0.9491 0.048 Uiso 1 1 calc R . .
C27 C 0.3382(3) -0.31763(17) 0.90929(13) 0.0372(7) Uani 1 1 d . . .
H27 H 0.2946 -0.3598 0.9243 0.045 Uiso 1 1 calc R . .
C28 C 0.2735(2) -0.25332(16) 0.87220(12) 0.0285(6) Uani 1 1 d . . .
H28 H 0.1858 -0.2519 0.8623 0.034 Uiso 1 1 calc R . .
C29 C 0.5361(2) -0.12418(19) 0.84610(15) 0.0381(7) Uani 1 1 d . . .
H29A H 0.6245 -0.1374 0.8585 0.057 Uiso 1 1 calc R . .
H29B H 0.5239 -0.0758 0.8714 0.057 Uiso 1 1 calc R . .
H29C H 0.5058 -0.1150 0.7950 0.057 Uiso 1 1 calc R . .
C30 C 0.1588(2) -0.13386(15) 0.77029(12) 0.0206(5) Uani 1 1 d . . .
H30 H 0.1204 -0.1850 0.7652 0.025 Uiso 1 1 calc R . .
C31 C 0.1688(3) -0.00102(19) 0.91686(16) 0.0465(8) Uani 1 1 d . . .
H31A H 0.2310 -0.0440 0.9323 0.056 Uiso 1 1 calc R . .
H31B H 0.0886 -0.0259 0.8921 0.056 Uiso 1 1 calc R . .
C32 C 0.1564(5) 0.0445(2) 0.9781(2) 0.0913(15) Uani 1 1 d . . .
H32A H 0.2083 0.0205 1.0224 0.110 Uiso 1 1 calc R . .
H32B H 0.0691 0.0445 0.9798 0.110 Uiso 1 1 calc R . .
C33 C 0.1988(3) 0.12845(18) 0.96953(15) 0.0395(7) Uani 1 1 d . . .
H33A H 0.2859 0.1367 0.9972 0.047 Uiso 1 1 calc R . .
H33B H 0.1457 0.1684 0.9843 0.047 Uiso 1 1 calc R . .
C34 C 0.1850(2) 0.13342(16) 0.89045(14) 0.0313(6) Uani 1 1 d . . .
H34A H 0.1006 0.1514 0.8646 0.038 Uiso 1 1 calc R . .
H34B H 0.2462 0.1710 0.8805 0.038 Uiso 1 1 calc R . .
C35 C 0.4315(2) 0.00295(17) 0.64551(14) 0.0333(6) Uani 1 1 d . . .
H35A H 0.5188 0.0055 0.6746 0.040 Uiso 1 1 calc R . .
H35B H 0.4000 0.0581 0.6349 0.040 Uiso 1 1 calc R . .
C36 C 0.4216(2) -0.04297(18) 0.57790(14) 0.0353(7) Uani 1 1 d . . .
H36A H 0.4961 -0.0353 0.5609 0.042 Uiso 1 1 calc R . .
H36B H 0.3471 -0.0271 0.5401 0.042 Uiso 1 1 calc R . .
C37 C 0.4117(3) -0.12856(18) 0.60184(15) 0.0409(7) Uani 1 1 d . . .
H37A H 0.3739 -0.1639 0.5612 0.049 Uiso 1 1 calc R . .
H37B H 0.4938 -0.1501 0.6277 0.049 Uiso 1 1 calc R . .
C38 C 0.3285(3) -0.11922(17) 0.65012(15) 0.0382(7) Uani 1 1 d . . .
H38A H 0.2403 -0.1226 0.6228 0.046 Uiso 1 1 calc R . .
H38B H 0.3458 -0.1614 0.6869 0.046 Uiso 1 1 calc R . .
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'
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 O2 174.04(6) . . ?
O1 Ca1 N1 94.90(7) . . ?
O2 Ca1 N1 91.06(7) . . ?
O1 Ca1 N4 88.95(6) . . ?
O2 Ca1 N4 85.20(6) . . ?
N1 Ca1 N4 169.60(6) . . ?
O1 Ca1 N3 87.34(6) . . ?
O2 Ca1 N3 90.37(6) . . ?
N1 Ca1 N3 114.15(6) . . ?
N4 Ca1 N3 56.29(6) . . ?
O1 Ca1 N2 89.60(6) . . ?
O2 Ca1 N2 93.58(6) . . ?
N1 Ca1 N2 56.41(6) . . ?
N4 Ca1 N2 133.43(6) . . ?
N3 Ca1 N2 169.78(7) . . ?
O1 Ca1 C15 93.69(6) . . ?
O2 Ca1 C15 91.48(6) . . ?
N1 Ca1 C15 28.38(6) . . ?
N4 Ca1 C15 161.07(6) . . ?
N3 Ca1 C15 142.51(7) . . ?
N2 Ca1 C15 28.07(6) . . ?
O1 Ca1 C30 89.67(6) . . ?
O2 Ca1 C30 85.73(6) . . ?
N1 Ca1 C30 141.78(6) . . ?
N4 Ca1 C30 28.33(6) . . ?
N3 Ca1 C30 28.06(6) . . ?
N2 Ca1 C30 161.76(7) . . ?
C15 Ca1 C30 169.87(7) . . ?
C31 O1 C34 108.1(2) . . ?
C31 O1 Ca1 124.18(16) . . ?
C34 O1 Ca1 127.60(14) . . ?
C35 O2 C38 109.13(19) . . ?
C35 O2 Ca1 124.57(15) . . ?
C38 O2 Ca1 126.13(14) . . ?
C15 N1 C1 118.2(2) . . ?
C15 N1 Ca1 92.07(14) . . ?
C1 N1 Ca1 149.08(15) . . ?
C15 N2 C8 117.6(2) . . ?
C15 N2 Ca1 91.22(13) . . ?
C8 N2 Ca1 148.64(16) . . ?
C30 N3 C16 118.6(2) . . ?
C30 N3 Ca1 92.10(13) . . ?
C16 N3 Ca1 145.65(15) . . ?
C30 N4 C23 118.8(2) . . ?
C30 N4 Ca1 91.79(14) . . ?
C23 N4 Ca1 149.27(15) . . ?
C6 C1 N1 122.4(2) . . ?
C6 C1 C2 119.1(2) . . ?
N1 C1 C2 118.5(2) . . ?
C3 C2 C1 118.0(2) . . ?
C3 C2 C7 120.9(2) . . ?
C1 C2 C7 121.1(2) . . ?
C4 C3 C2 122.5(2) . . ?
C3 C4 C5 119.7(2) . . ?
C6 C5 C4 119.2(3) . . ?
C5 C6 C1 121.5(2) . . ?
C13 C8 C9 119.3(2) . . ?
C13 C8 N2 122.2(2) . . ?
C9 C8 N2 118.5(2) . . ?
C10 C9 C8 118.4(2) . . ?
C10 C9 C14 120.6(2) . . ?
C8 C9 C14 121.0(2) . . ?
C11 C10 C9 122.0(2) . . ?
C12 C11 C10 119.6(2) . . ?
C11 C12 C13 119.8(2) . . ?
C8 C13 C12 121.1(2) . . ?
N2 C15 N1 120.1(2) . . ?
N2 C15 Ca1 60.71(12) . . ?
N1 C15 Ca1 59.54(13) . . ?
C21 C16 N3 122.8(2) . . ?
C21 C16 C17 119.2(2) . . ?
N3 C16 C17 117.9(2) . . ?
C18 C17 C16 118.3(2) . . ?
C18 C17 C22 120.9(2) . . ?
C16 C17 C22 120.9(2) . . ?
C19 C18 C17 121.9(2) . . ?
C18 C19 C20 119.7(2) . . ?
C19 C20 C21 119.4(3) . . ?
C20 C21 C16 121.3(2) . . ?
C28 C23 N4 123.5(2) . . ?
C28 C23 C24 118.6(2) . . ?
N4 C23 C24 117.8(2) . . ?
C25 C24 C23 118.6(2) . . ?
C25 C24 C29 121.0(2) . . ?
C23 C24 C29 120.5(2) . . ?
C26 C25 C24 121.6(2) . . ?
C27 C26 C25 119.7(3) . . ?
C26 C27 C28 120.3(3) . . ?
C27 C28 C23 121.2(2) . . ?
N3 C30 N4 119.4(2) . . ?
N3 C30 Ca1 59.84(12) . . ?
N4 C30 Ca1 59.88(12) . . ?
O1 C31 C32 107.9(3) . . ?
C31 C32 C33 106.8(3) . . ?
C32 C33 C34 102.6(3) . . ?
O1 C34 C33 104.6(2) . . ?
O2 C35 C36 105.6(2) . . ?
C35 C36 C37 101.6(2) . . ?
C38 C37 C36 101.9(2) . . ?
O2 C38 C37 105.5(2) . . ?
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 2.3668(16) . ?
Ca1 O2 2.3688(17) . ?
Ca1 N1 2.415(2) . ?
Ca1 N4 2.425(2) . ?
Ca1 N3 2.4244(19) . ?
Ca1 N2 2.442(2) . ?
Ca1 C15 2.799(2) . ?
Ca1 C30 2.802(2) . ?
O1 C31 1.436(3) . ?
O1 C34 1.438(3) . ?
O2 C35 1.445(3) . ?
O2 C38 1.454(3) . ?
N1 C15 1.332(3) . ?
N1 C1 1.406(3) . ?
N2 C15 1.317(3) . ?
N2 C8 1.412(3) . ?
N3 C30 1.319(3) . ?
N3 C16 1.407(3) . ?
N4 C30 1.330(3) . ?
N4 C23 1.402(3) . ?
C1 C6 1.393(4) . ?
C1 C2 1.418(3) . ?
C2 C3 1.388(3) . ?
C2 C7 1.500(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.384(3) . ?
C5 C6 1.393(3) . ?
C8 C13 1.395(3) . ?
C8 C9 1.409(3) . ?
C9 C10 1.397(3) . ?
C9 C14 1.497(3) . ?
C10 C11 1.381(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.392(3) . ?
C16 C21 1.394(3) . ?
C16 C17 1.411(3) . ?
C17 C18 1.391(3) . ?
C17 C22 1.498(4) . ?
C18 C19 1.386(4) . ?
C19 C20 1.382(4) . ?
C20 C21 1.389(3) . ?
C23 C28 1.397(3) . ?
C23 C24 1.413(3) . ?
C24 C25 1.397(4) . ?
C24 C29 1.504(4) . ?
C25 C26 1.385(4) . ?
C26 C27 1.367(4) . ?
C27 C28 1.388(4) . ?
C31 C32 1.461(4) . ?
C32 C33 1.507(5) . ?
C33 C34 1.521(4) . ?
C35 C36 1.512(4) . ?
C36 C37 1.521(4) . ?
C37 C38 1.511(4) . ?
