#------------------------------------------------------------------------------
#$Date: 2016-06-17 01:44:05 +0300 (Fri, 17 Jun 2016) $
#$Revision: 183564 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/50/4125039.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_4125039
loop_
_publ_author_name
'Hill, Joshua A.'
'Thompson, Amber L.'
'Goodwin, Andrew L.'
_publ_section_title
;
 Dicyanometallates as Model Extended Frameworks.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5886
_journal_page_last               5896
_journal_paper_doi               10.1021/jacs.5b13446
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C6 Au3 Mn N6, C36 H30 N P2'
_chemical_formula_sum            'C42 H30 Au3 Mn N7 P2'
_chemical_formula_weight         1340.52
_chemical_name_systematic
;
bis(triphenylphosphoranylidene)ammonium manganese dicyanoaurate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-12-03
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 92.5382(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7035(3)
_cell_length_b                   12.5777(3)
_cell_length_c                   20.6707(4)
_cell_measurement_reflns_used    5155
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4338.48(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37786
_diffrn_reflns_theta_full        26.939
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         5.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.509
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.8163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.97
_refine_diff_density_min         -1.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9881
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4947
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.0009386
_refine_ls_shift/su_mean         0.0000259
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² +12.05P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0717
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0717
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                4065
_reflns_number_total             4947
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0435
_oxford_refine_ls_scale          0.065186(9)
_oxford_reflns_number_all        4947
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 050jah13
_cod_data_source_file            ja5b13446_si_001.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4125033--4125042.cif.
;
_cod_original_sg_symbol_H-M      'I 2/a '
_cod_original_formula_sum        'C42 H30 Au3 Mn1 N7 P2'
_cod_database_code               4125039
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z+1/2
-x+1/2,-y+1/2,-z+1/2
-x+1/2,y,-z
x+1/2,-y,z
-x+1,y+1/2,-z+1/2
x+1,-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Au1 Au 0.479493(10) 0.529905(15) 0.276457(9) 0.0353 1.0000 Uani . .
Au2 Au 0.2500 0.33584(2) 0.0000 0.0319 1.0000 Uani S T
Mn3 Mn 0.2500 0.2500 0.2500 0.0231 1.0000 Uani S .
C4 C 0.3820(3) 0.4412(4) 0.2817(2) 0.0369 1.0000 Uani . .
N5 N 0.3282(2) 0.3860(3) 0.2830(2) 0.0386 1.0000 Uani . .
C6 C 0.2543(3) 0.3283(4) 0.0957(2) 0.0341 1.0000 Uani . .
N7 N 0.2547(2) 0.3135(4) 0.15026(19) 0.0390 1.0000 Uani . .
C8 C 0.4201(3) 0.1126(4) 0.2307(2) 0.0376 1.0000 Uani . .
N9 N 0.3615(2) 0.1578(3) 0.2354(2) 0.0370 1.0000 Uani . .
N10 N 0.2500 0.8028(4) 0.5000 0.0266 1.0000 Uani S T
P11 P 0.33494(6) 0.76390(9) 0.48047(6) 0.0277 1.0000 Uani . .
H12 H 0.2374 0.8531 0.3785 0.0561 1.0000 Uiso R .
C13 C 0.4105(3) 0.8341(4) 0.5285(2) 0.0307 1.0000 Uani . .
C14 C 0.3971(3) 0.9385(4) 0.5453(3) 0.0387 1.0000 Uani . .
C15 C 0.4542(3) 0.9945(4) 0.5821(3) 0.0460 1.0000 Uani . .
C16 C 0.5245(3) 0.9449(5) 0.6030(3) 0.0429 1.0000 Uani . .
C17 C 0.5376(3) 0.8417(5) 0.5873(3) 0.0548 1.0000 Uani . .
C18 C 0.4817(3) 0.7848(5) 0.5496(3) 0.0462 1.0000 Uani . .
C19 C 0.3521(3) 0.6244(4) 0.4934(2) 0.0315 1.0000 Uani . .
C20 C 0.3496(3) 0.5865(5) 0.5569(3) 0.0481 1.0000 Uani . .
C21 C 0.3578(4) 0.4782(5) 0.5694(3) 0.0574 1.0000 Uani . .
C22 C 0.3696(3) 0.4093(4) 0.5194(3) 0.0500 1.0000 Uani . .
C23 C 0.3711(4) 0.4457(5) 0.4565(3) 0.0526 1.0000 Uani . .
C24 C 0.3631(3) 0.5528(4) 0.4443(3) 0.0448 1.0000 Uani . .
C25 C 0.3493(3) 0.7941(4) 0.3967(2) 0.0317 1.0000 Uani . .
C26 C 0.4213(3) 0.7758(4) 0.3679(2) 0.0398 1.0000 Uani . .
C27 C 0.4306(4) 0.8017(4) 0.3034(3) 0.0495 1.0000 Uani . .
C28 C 0.3684(4) 0.8456(5) 0.2676(3) 0.0540 1.0000 Uani . .
C29 C 0.2969(4) 0.8649(5) 0.2955(3) 0.0583 1.0000 Uani . .
C30 C 0.2858(3) 0.8391(4) 0.3597(2) 0.0451 1.0000 Uani . .
H131 H 0.3643 0.5767 0.4007 0.0551 1.0000 Uiso R .
H141 H 0.3778 0.3970 0.4220 0.0659 1.0000 Uiso R .
H151 H 0.3763 0.3369 0.5284 0.0619 1.0000 Uiso R .
H161 H 0.3563 0.4535 0.6121 0.0700 1.0000 Uiso R .
H171 H 0.3451 0.6344 0.5907 0.0596 1.0000 Uiso R .
H191 H 0.3480 0.9721 0.5312 0.0493 1.0000 Uiso R .
H201 H 0.4465 1.0649 0.5925 0.0566 1.0000 Uiso R .
H211 H 0.5634 0.9839 0.6278 0.0530 1.0000 Uiso R .
H221 H 0.5850 0.8087 0.6019 0.0670 1.0000 Uiso R .
H231 H 0.4913 0.7136 0.5386 0.0571 1.0000 Uiso R .
H261 H 0.2533 0.8950 0.2709 0.0711 1.0000 Uiso R .
H271 H 0.3740 0.8623 0.2246 0.0667 1.0000 Uiso R .
H281 H 0.4795 0.7903 0.2844 0.0600 1.0000 Uiso R .
H291 H 0.4649 0.7469 0.3933 0.0499 1.0000 Uiso R .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Au -2.0133 8.8022 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956
12.0658 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C8 7_555 Au1 C4 . 177.2(2) yes
C6 5_555 Au2 C6 . 174.5(3) yes
N7 4_555 Mn3 N9 4_555 89.84(15) yes
N7 4_555 Mn3 N5 4_555 87.92(15) yes
N9 4_555 Mn3 N5 4_555 87.65(15) yes
N7 4_555 Mn3 N5 . 92.08(15) yes
N9 4_555 Mn3 N5 . 92.35(15) yes
N5 4_555 Mn3 N5 . 179.995 yes
N7 4_555 Mn3 N7 . 179.995 yes
N9 4_555 Mn3 N7 . 90.16(15) yes
N5 4_555 Mn3 N7 . 92.08(15) yes
N5 . Mn3 N7 . 87.92(15) yes
N7 4_555 Mn3 N9 . 90.16(15) yes
N9 4_555 Mn3 N9 . 179.995 yes
N5 4_555 Mn3 N9 . 92.35(15) yes
N5 . Mn3 N9 . 87.65(15) yes
N7 . Mn3 N9 . 89.84(15) yes
Au1 . C4 N5 . 176.2(5) yes
Mn3 . N5 C4 . 155.6(4) yes
Au2 . C6 N7 . 173.2(5) yes
Mn3 . N7 C6 . 168.0(4) yes
Au1 7_545 C8 N9 . 178.2(5) yes
Mn3 . N9 C8 . 176.7(4) yes
P11 5_556 N10 P11 . 143.7(4) yes
N10 . P11 C13 . 108.9(2) yes
N10 . P11 C19 . 114.0(2) yes
C13 . P11 C19 . 107.1(2) yes
N10 . P11 C25 . 110.01(17) yes
C13 . P11 C25 . 107.9(2) yes
C19 . P11 C25 . 108.8(2) yes
P11 . C13 C14 . 119.2(3) yes
P11 . C13 C18 . 121.4(4) yes
C14 . C13 C18 . 119.4(4) yes
C13 . C14 C15 . 120.5(5) yes
C13 . C14 H191 . 119.4 no
C15 . C14 H191 . 120.1 no
C14 . C15 C16 . 119.8(5) yes
C14 . C15 H201 . 121.1 no
C16 . C15 H201 . 119.1 no
C15 . C16 C17 . 120.0(5) yes
C15 . C16 H211 . 119.2 no
C17 . C16 H211 . 120.8 no
C16 . C17 C18 . 121.1(5) yes
C16 . C17 H221 . 119.4 no
C18 . C17 H221 . 119.5 no
C13 . C18 C17 . 119.3(5) yes
C13 . C18 H231 . 120.0 no
C17 . C18 H231 . 120.7 no
P11 . C19 C20 . 117.5(4) yes
P11 . C19 C24 . 123.8(4) yes
C20 . C19 C24 . 118.7(5) yes
C19 . C20 C21 . 120.0(5) yes
C19 . C20 H171 . 119.5 no
C21 . C20 H171 . 120.4 no
C20 . C21 C22 . 119.7(5) yes
C20 . C21 H161 . 119.6 no
C22 . C21 H161 . 120.7 no
C21 . C22 C23 . 120.7(5) yes
C21 . C22 H151 . 119.1 no
C23 . C22 H151 . 120.2 no
C22 . C23 C24 . 119.5(6) yes
C22 . C23 H141 . 120.1 no
C24 . C23 H141 . 120.4 no
C23 . C24 C19 . 121.4(5) yes
C23 . C24 H131 . 118.5 no
C19 . C24 H131 . 120.1 no
P11 . C25 C26 . 122.3(4) yes
P11 . C25 C30 . 118.7(4) yes
C26 . C25 C30 . 119.0(5) yes
C25 . C26 C27 . 120.7(5) yes
C25 . C26 H291 . 119.0 no
C27 . C26 H291 . 120.2 no
C26 . C27 C28 . 119.9(5) yes
C26 . C27 H281 . 120.5 no
C28 . C27 H281 . 119.6 no
C27 . C28 C29 . 120.1(5) yes
C27 . C28 H271 . 120.4 no
C29 . C28 H271 . 119.5 no
C28 . C29 C30 . 121.1(6) yes
C28 . C29 H261 . 120.5 no
C30 . C29 H261 . 118.4 no
C25 . C30 C29 . 119.2(5) yes
C25 . C30 H12 . 120.1 no
C29 . C30 H12 . 120.6 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Au1 C8 7_555 1.985(5) yes
Au1 C4 . 1.981(5) yes
Au2 C6 5_555 1.980(5) yes
Au2 C6 . 1.980(5) yes
Mn3 N7 4_555 2.216(4) yes
Mn3 N9 4_555 2.226(4) yes
Mn3 N5 4_555 2.240(4) yes
Mn3 N5 . 2.240(4) yes
Mn3 N7 . 2.216(4) yes
Mn3 N9 . 2.226(4) yes
C4 N5 . 1.137(6) yes
C6 N7 . 1.142(6) yes
C8 N9 . 1.139(6) yes
N10 P11 5_556 1.571(2) yes
N10 P11 . 1.571(2) yes
P11 C13 . 1.802(4) yes
P11 C19 . 1.796(5) yes
P11 C25 . 1.799(5) yes
H12 C30 . 0.930 no
C13 C14 . 1.378(7) yes
C13 C18 . 1.395(6) yes
C14 C15 . 1.386(7) yes
C14 H191 . 0.958 no
C15 C16 . 1.382(7) yes
C15 H201 . 0.922 no
C16 C17 . 1.357(8) yes
C16 H211 . 0.947 no
C17 C18 . 1.388(7) yes
C17 H221 . 0.932 no
C18 H231 . 0.938 no
C19 C20 . 1.400(7) yes
C19 C24 . 1.375(7) yes
C20 C21 . 1.392(8) yes
C20 H171 . 0.928 no
C21 C22 . 1.371(9) yes
C21 H161 . 0.937 no
C22 C23 . 1.379(8) yes
C22 H151 . 0.935 no
C23 C24 . 1.375(7) yes
C23 H141 . 0.951 no
C24 H131 . 0.951 no
C25 C26 . 1.383(6) yes
C25 C30 . 1.399(7) yes
C26 C27 . 1.388(7) yes
C26 H291 . 0.952 no
C27 C28 . 1.366(9) yes
C27 H281 . 0.933 no
C28 C29 . 1.370(9) yes
C28 H271 . 0.922 no
C29 C30 . 1.388(8) yes
C29 H261 . 0.948 no
