#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:01:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179274 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319465.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_4319465
loop_
_publ_author_name
'Patricia M. van der Werff'
'Stuart R. Batten'
'Paul Jensen'
'Boujemaa Moubaraki'
'Keith S. Murray'
_publ_contact_author
;
     Prof. K.S. Murray
     Department of Chemistry
     PO Box 23
     Monash University 3800
     AUSTRALIA
;
_publ_contact_author_email       'Keith.S.Murray@sci.monash.edu.au '
_publ_contact_author_fax         ' +61 3 9905 4597 '
_publ_contact_author_phone       ' +61 3 9905 4512 '
_publ_section_title
;
 Cation Templation of Anionic Metal Dicyanamide Networks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1718
_journal_page_last               1722
_journal_paper_doi               10.1021/ic000978x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         (Ph4P)(Mn(dca)3)
_chemical_formula_sum            'C30 H20 Mn N9 P'
_chemical_formula_weight         592.46
_chemical_name_common            (Ph4P)(Mn(dca)3)
_chemical_name_systematic
;
  tetraphenylphosphonium manganese(II) tris(dicyanamide)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 98.731(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2564(3)
_cell_length_b                   7.5742(1)
_cell_length_c                   14.2386(3)
_cell_measurement_temperature    123(2)
_cell_volume                     1413.08(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Phi-scans and 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  0.025
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19791
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   Face-indexed
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0293
_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)+(0.0173P)²+0.7780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                3207
_reflns_number_total             3574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000978x_1.cif
_cod_data_source_block           Ph4Pmndca3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319465
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
Mn1 Mn 0.2500 0.46057(3) 0.2500 0.01442(7) Uani 1 2 d S . .
P1 P -0.2500 0.28106(6) 0.2500 0.01619(10) Uani 1 2 d S . .
N1 N 0.32002(9) 0.24508(14) 0.17625(8) 0.0230(2) Uani 1 1 d . . .
N2 N 0.35615(10) -0.04057(14) 0.10636(8) 0.0274(3) Uani 1 1 d . . .
N3 N 0.31922(9) -0.32718(14) 0.17459(8) 0.0250(2) Uani 1 1 d . . .
N7 N 0.11723(9) 0.46347(16) 0.12969(9) 0.0300(3) Uani 1 1 d . . .
N8 N -0.05862(18) 0.4666(4) 0.04061(16) 0.0308(5) Uani 0.50 1 d P . .
C1 C 0.33451(10) 0.10729(16) 0.14610(8) 0.0184(2) Uani 1 1 d . . .
C2 C 0.33397(10) -0.18919(16) 0.14570(9) 0.0188(2) Uani 1 1 d . . .
C5 C 0.0352(2) 0.4658(3) 0.08417(18) 0.0202(5) Uani 0.50 1 d P . .
C6 C -0.0864(2) 0.5029(3) -0.0493(2) 0.0205(5) Uani 0.50 1 d P . .
C7 C -0.17070(9) 0.14158(16) 0.19001(8) 0.0178(2) Uani 1 1 d . . .
C8 C -0.06512(10) 0.16339(19) 0.20128(9) 0.0240(3) Uani 1 1 d . . .
H8 H -0.0332 0.2547 0.2409 0.029 Uiso 1 1 calc R . .
C9 C -0.00704(11) 0.0507(2) 0.15422(10) 0.0283(3) Uani 1 1 d . . .
H9 H 0.0649 0.0652 0.1616 0.034 Uiso 1 1 calc R . .
C10 C -0.05336(11) -0.08259(18) 0.09660(10) 0.0254(3) Uani 1 1 d . . .
H10 H -0.0131 -0.1594 0.0648 0.030 Uiso 1 1 calc R . .
C11 C -0.15858(11) -0.10428(18) 0.08515(10) 0.0267(3) Uani 1 1 d . . .
H11 H -0.1902 -0.1956 0.0454 0.032 Uiso 1 1 calc R . .
C12 C -0.21728(10) 0.00722(18) 0.13173(10) 0.0237(3) Uani 1 1 d . . .
H12 H -0.2892 -0.0076 0.1241 0.028 Uiso 1 1 calc R . .
C13 C -0.32522(9) 0.42850(16) 0.16908(9) 0.0179(2) Uani 1 1 d . . .
C14 C -0.32346(10) 0.42329(17) 0.07169(9) 0.0200(3) Uani 1 1 d . . .
H14 H -0.2889 0.3309 0.0446 0.024 Uiso 1 1 calc R . .
C15 C -0.37320(11) 0.55562(17) 0.01447(9) 0.0246(3) Uani 1 1 d . . .
H15 H -0.3733 0.5527 -0.0522 0.029 Uiso 1 1 calc R . .
C16 C -0.42249(10) 0.69136(17) 0.05423(10) 0.0252(3) Uani 1 1 d . . .
H16 H -0.4551 0.7821 0.0147 0.030 Uiso 1 1 calc R . .
C17 C -0.42465(10) 0.69609(17) 0.15127(10) 0.0241(3) Uani 1 1 d . . .
H17 H -0.4592 0.7889 0.1780 0.029 Uiso 1 1 calc R . .
C18 C -0.37617(10) 0.56482(17) 0.20895(9) 0.0226(3) Uani 1 1 d . . .
H18 H -0.3775 0.5672 0.2755 0.027 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
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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'
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
N3 Mn1 N3 86.58(6) 1_565 2_565 ?
N3 Mn1 N1 94.06(4) 1_565 . ?
N3 Mn1 N1 179.15(4) 2_565 . ?
N3 Mn1 N1 179.15(4) 1_565 2 ?
N3 Mn1 N1 94.06(4) 2_565 2 ?
N1 Mn1 N1 85.30(6) . 2 ?
N3 Mn1 N7 87.57(4) 1_565 . ?
N3 Mn1 N7 91.62(5) 2_565 . ?
N1 Mn1 N7 88.97(4) . . ?
N1 Mn1 N7 91.85(4) 2 . ?
N3 Mn1 N7 91.61(5) 1_565 2 ?
N3 Mn1 N7 87.57(4) 2_565 2 ?
N1 Mn1 N7 91.85(4) . 2 ?
N1 Mn1 N7 88.97(4) 2 2 ?
N7 Mn1 N7 178.89(6) . 2 ?
C13 P1 C13 103.03(8) 2_455 . ?
C13 P1 C7 111.67(5) 2_455 2_455 ?
C13 P1 C7 111.30(6) . 2_455 ?
C13 P1 C7 111.30(6) 2_455 . ?
C13 P1 C7 111.67(5) . . ?
C7 P1 C7 107.91(8) 2_455 . ?
C1 N1 Mn1 160.93(11) . . ?
C1 N2 C2 118.23(11) . . ?
C2 N3 Mn1 160.15(10) . 1_545 ?
C5 N7 C6 46.41(17) . 3_565 ?
C5 N7 Mn1 164.47(17) . . ?
C6 N7 Mn1 148.14(17) 3_565 . ?
C5 N8 C6 125.0(2) . . ?
C5 N8 C5 99.50(19) . 3_565 ?
C6 N8 C5 25.56(15) . 3_565 ?
C5 N8 C6 25.38(15) . 3_565 ?
C6 N8 C6 99.68(18) . 3_565 ?
C5 N8 C6 74.13(14) 3_565 3_565 ?
N1 C1 N2 174.34(13) . . ?
N3 C2 N2 173.87(13) . . ?
C6 C5 N7 67.1(3) 3_565 . ?
C6 C5 N8 117.7(3) 3_565 . ?
N7 C5 N8 175.1(3) . . ?
C6 C5 N8 37.3(2) 3_565 3_565 ?
N7 C5 N8 104.4(2) . 3_565 ?
N8 C5 N8 80.50(18) . 3_565 ?
C5 C6 N7 66.5(3) 3_565 3_565 ?
C5 C6 N8 117.2(3) 3_565 . ?
N7 C6 N8 176.2(3) 3_565 . ?
C5 C6 N8 36.9(2) 3_565 3_565 ?
N7 C6 N8 103.4(2) 3_565 3_565 ?
N8 C6 N8 80.32(18) . 3_565 ?
C8 C7 C12 120.03(12) . . ?
C8 C7 P1 121.71(10) . . ?
C12 C7 P1 118.26(10) . . ?
C9 C8 C7 119.49(12) . . ?
C10 C9 C8 120.39(13) . . ?
C9 C10 C11 120.19(12) . . ?
C12 C11 C10 119.94(12) . . ?
C11 C12 C7 119.96(12) . . ?
C14 C13 C18 120.47(12) . . ?
C14 C13 P1 122.05(10) . . ?
C18 C13 P1 116.99(9) . . ?
C13 C14 C15 118.99(12) . . ?
C16 C15 C14 120.40(12) . . ?
C15 C16 C17 120.60(12) . . ?
C18 C17 C16 119.65(12) . . ?
C17 C18 C13 119.88(12) . . ?
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
Mn1 N3 2.2087(11) 1_565 ?
Mn1 N3 2.2087(11) 2_565 ?
Mn1 N1 2.2190(11) . ?
Mn1 N1 2.2190(11) 2 ?
Mn1 N7 2.2621(11) . ?
Mn1 N7 2.2622(11) 2 ?
P1 C13 1.7945(13) 2_455 ?
P1 C13 1.7945(13) . ?
P1 C7 1.7953(12) 2_455 ?
P1 C7 1.7954(12) . ?
N1 C1 1.1556(16) . ?
N2 C1 1.3061(16) . ?
N2 C2 1.3105(16) . ?
N3 C2 1.1507(16) . ?
N3 Mn1 2.2087(11) 1_545 ?
N7 C5 1.178(3) . ?
N7 C6 1.184(3) 3_565 ?
N8 C5 1.303(4) . ?
N8 C6 1.306(3) . ?
N8 C5 1.919(4) 3_565 ?
N8 C6 1.922(4) 3_565 ?
C5 C6 0.931(4) 3_565 ?
C5 N8 1.919(4) 3_565 ?
C6 C5 0.931(4) 3_565 ?
C6 N7 1.184(3) 3_565 ?
C6 N8 1.922(4) 3_565 ?
C7 C8 1.3942(18) . ?
C7 C12 1.3965(18) . ?
C8 C9 1.3881(19) . ?
C9 C10 1.384(2) . ?
C10 C11 1.389(2) . ?
C11 C12 1.3840(19) . ?
C13 C14 1.3909(17) . ?
C13 C18 1.4003(17) . ?
C14 C15 1.3929(18) . ?
C15 C16 1.385(2) . ?
C16 C17 1.387(2) . ?
C17 C18 1.3841(18) . ?
