#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:37:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179980 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/74/7027466.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027466
loop_
_publ_author_name
'McAdam, C. John'
'Brunton, Jason J.'
'Robinson, Brian H.'
'Simpson, Jim'
_publ_section_title
;
 Ferrocenylethynylnaphthalenes and acenaphthylenes; communication between
 ferrocenyl and cluster redox centres
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2487
_journal_paper_doi               10.1039/a903003d
_journal_year                    1999
_chemical_formula_sum            'C46 H52 Co4 O20 P4'
_chemical_formula_weight         1284.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.515(5)
_cell_length_b                   13.242(6)
_cell_length_c                   30.181(7)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      10.0
_cell_volume                     5401(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'SHELXTL-PC (Sheldrick 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Siemens R3m/V'
_diffrn_measurement_method       'ω 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  0.1563
_diffrn_reflns_av_sigmaI/netI    0.3682
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            7916
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        '< 1%'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  0.9236
_exptl_absorpt_correction_T_min  0.0788
_exptl_absorpt_correction_type   'empirical \y scans'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.948
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4753
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.2202
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0446P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                1552
_reflns_number_total             4753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903003dsup1.cif
_cod_data_source_block           compound22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5402(3)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7027466
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.43615(11) 0.24179(10) 0.39250(4) 0.0239(4) Uani 1 d . . .
C11 C 0.3130(10) 0.2515(10) 0.4107(3) 0.045(3) Uani 1 d . . .
O11 O 0.2298(7) 0.2458(7) 0.4223(2) 0.056(2) Uani 1 d . . .
C12 C 0.4603(9) 0.3331(8) 0.3523(3) 0.036(3) Uani 1 d . . .
O12 O 0.4799(6) 0.3931(5) 0.3248(2) 0.053(2) Uani 1 d . . .
P1 P 0.5026(2) 0.3206(2) 0.44657(8) 0.0254(7) Uani 1 d . . .
O13 O 0.5035(6) 0.2759(5) 0.49520(19) 0.0324(18) Uani 1 d . . .
C13 C 0.4149(8) 0.2482(7) 0.5170(3) 0.038(3) Uani 1 d . . .
H13A H 0.4285 0.1958 0.5381 0.057 Uiso 1 calc R . .
H13B H 0.3679 0.2242 0.4956 0.057 Uiso 1 calc R . .
H13C H 0.3881 0.3059 0.5321 0.057 Uiso 1 calc R . .
O14 O 0.4566(5) 0.4295(5) 0.45984(19) 0.035(2) Uani 1 d . . .
C14 C 0.4489(8) 0.5076(8) 0.4266(3) 0.045(3) Uani 1 d . . .
H14A H 0.4273 0.5693 0.4402 0.068 Uiso 1 calc R . .
H14B H 0.4019 0.4875 0.4044 0.068 Uiso 1 calc R . .
H14C H 0.5124 0.5179 0.4130 0.068 Uiso 1 calc R . .
O15 O 0.6166(5) 0.3404(5) 0.43849(19) 0.0299(19) Uani 1 d . . .
C15 C 0.6750(7) 0.3945(8) 0.4704(3) 0.046(3) Uani 1 d . . .
H15A H 0.7404 0.4049 0.4588 0.069 Uiso 1 calc R . .
H15B H 0.6790 0.3561 0.4973 0.069 Uiso 1 calc R . .
H15C H 0.6448 0.4587 0.4764 0.069 Uiso 1 calc R . .
Co2 Co 0.41132(11) 0.09703(10) 0.34390(4) 0.0296(4) Uani 1 d . . .
C21 C 0.4343(10) 0.1548(8) 0.2931(3) 0.049(3) Uani 1 d . . .
O21 O 0.4486(8) 0.1952(6) 0.2585(2) 0.085(4) Uani 1 d . . .
C22 C 0.2820(11) 0.0825(9) 0.3451(3) 0.045(4) Uani 1 d . . .
O22 O 0.1950(6) 0.0788(7) 0.3431(3) 0.060(3) Uani 1 d . . .
P2 P 0.4373(3) -0.0546(2) 0.32328(10) 0.0576(11) Uani 1 d . . .
O23A O 0.5479(12) -0.0872(10) 0.3080(5) 0.047(5) Uani 0.55(2) d PU A 1
O23B O 0.492(2) -0.0830(19) 0.2832(9) 0.102(9) Uani 0.45(2) d PU A 2
C23 C 0.5921(12) -0.0318(10) 0.2716(4) 0.089(5) Uani 1 d . . .
H23A H 0.6566 -0.0587 0.2654 0.134 Uiso 0.55(2) calc PR A 1
H23B H 0.5977 0.0382 0.2794 0.134 Uiso 0.55(2) calc PR A 1
H23C H 0.5511 -0.0383 0.2457 0.134 Uiso 0.55(2) calc PR A 1
H23D H 0.6171 -0.0596 0.2444 0.134 Uiso 0.45(2) calc PR A 2
H23E H 0.6388 -0.0436 0.2950 0.134 Uiso 0.45(2) calc PR A 2
H23F H 0.5821 0.0395 0.2681 0.134 Uiso 0.45(2) calc PR A 2
O24 O 0.3531(12) -0.0872(9) 0.2889(5) 0.181(7) Uani 1 d . A 2
C24 C 0.3298(12) -0.1663(13) 0.2700(5) 0.142(8) Uani 1 d . A 2
H24A H 0.3170 -0.1528 0.2393 0.213 Uiso 1 calc R A 2
H24B H 0.2714 -0.1936 0.2836 0.213 Uiso 1 calc R A 2
H24C H 0.3829 -0.2141 0.2725 0.213 Uiso 1 calc R A 2
O25A O 0.471(2) -0.1326(16) 0.3634(7) 0.086(7) Uani 0.55(2) d PU A 1
C25A C 0.473(3) -0.199(3) 0.3834(12) 0.111(12) Uani 0.55(2) d PU A 1
H25A H 0.5227 -0.1919 0.4059 0.167 Uiso 0.55(2) calc PR A 1
H25B H 0.4888 -0.2564 0.3651 0.167 Uiso 0.55(2) calc PR A 1
H25C H 0.4097 -0.2092 0.3970 0.167 Uiso 0.55(2) calc PR A 1
O25B O 0.4068(16) -0.1422(13) 0.3572(5) 0.038(6) Uani 0.45(2) d PU A 2
C25B C 0.4795(19) -0.2359(19) 0.3595(9) 0.043(7) Uani 0.45(2) d PU A 2
H25D H 0.4543 -0.2846 0.3802 0.064 Uiso 0.45(2) calc PR A 2
H25E H 0.5437 -0.2137 0.3689 0.064 Uiso 0.45(2) calc PR A 2
H25F H 0.4845 -0.2664 0.3307 0.064 Uiso 0.45(2) calc PR A 2
C1 C 0.5297(7) 0.1359(7) 0.3787(3) 0.018(2) Uani 1 d U . .
C2 C 0.4586(7) 0.0969(7) 0.4048(2) 0.015(2) Uani 1 d U . .
C16 C 0.6342(8) 0.1218(7) 0.3658(3) 0.028(3) Uani 1 d U . .
C17 C 0.6881(9) 0.1975(8) 0.3428(3) 0.036(3) Uani 1 d . . .
H17 H 0.6587 0.2600 0.3378 0.044 Uiso 1 calc R . .
C18 C 0.7823(9) 0.1806(11) 0.3276(4) 0.061(4) Uani 1 d . . .
H18 H 0.8145 0.2306 0.3115 0.074 Uiso 1 calc R . .
C19 C 0.8304(10) 0.0900(11) 0.3361(4) 0.067(4) Uani 1 d . . .
H19 H 0.8936 0.0781 0.3251 0.081 Uiso 1 calc R . .
C110 C 0.7824(9) 0.0179(9) 0.3613(3) 0.048(4) Uani 1 d . . .
H110 H 0.8153 -0.0413 0.3690 0.058 Uiso 1 calc R . .
C111 C 0.6856(8) 0.0329(8) 0.3752(3) 0.029(3) Uani 1 d . . .
H111 H 0.6541 -0.0178 0.3912 0.035 Uiso 1 calc R . .
C26 C 0.3284(8) -0.0676(7) 0.4876(3) 0.025(2) Uani 1 d U . .
H26 H 0.2671 -0.0990 0.4901 0.030 Uiso 1 calc R . .
C27 C 0.3518(8) -0.0121(7) 0.4492(3) 0.024(2) Uani 1 d U . .
H27 H 0.3066 -0.0081 0.4260 0.028 Uiso 1 calc R . .
C28 C 0.4420(8) 0.0362(6) 0.4459(3) 0.020(2) Uani 1 d U . .
C29 C 0.5124(8) 0.0292(6) 0.4806(2) 0.016(2) Uani 1 d U . .
C210 C 0.6048(7) 0.0753(6) 0.4788(3) 0.020(2) Uani 1 d U . .
H210 H 0.6215 0.1126 0.4538 0.024 Uiso 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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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
C12 Co1 C11 110.1(5) . . ?
C12 Co1 C1 103.4(4) . . ?
C11 Co1 C1 137.7(5) . . ?
C12 Co1 C2 140.8(4) . . ?
C11 Co1 C2 99.1(5) . . ?
C1 Co1 C2 40.2(3) . . ?
C11 Co1 P1 97.1(4) . . y
C12 Co1 P1 96.5(3) . . y
C1 Co1 P1 104.1(3) . . ?
C2 Co1 P1 105.4(2) . . ?
C12 Co1 Co2 98.8(3) . . ?
C11 Co1 Co2 96.6(4) . . ?
C1 Co1 Co2 52.4(3) . . ?
C2 Co1 Co2 51.0(2) . . ?
P1 Co1 Co2 154.47(10) . . y
O11 C11 Co1 172.1(13) . . y
O12 C12 Co1 177.5(10) . . y
O13 P1 O15 101.4(4) . . ?
O13 P1 O14 96.1(3) . . ?
O15 P1 O14 105.3(4) . . ?
O13 P1 Co1 122.0(3) . . ?
O15 P1 Co1 111.9(3) . . ?
O14 P1 Co1 117.6(3) . . ?
C13 O13 P1 121.4(6) . . ?
C14 O14 P1 119.6(6) . . ?
C15 O15 P1 121.0(6) . . ?
C21 Co2 C22 104.1(5) . . ?
C21 Co2 C2 140.7(5) . . ?
C22 Co2 C2 107.8(4) . . ?
C21 Co2 C1 102.0(5) . . ?
C22 Co2 C1 145.0(4) . . ?
C2 Co2 C1 40.1(3) . . ?
C21 Co2 P2 97.3(4) . . y
C22 Co2 P2 93.8(4) . . y
C2 Co2 P2 102.8(3) . . ?
C1 Co2 P2 105.4(3) . . ?
C21 Co2 Co1 99.2(3) . . ?
C22 Co2 Co1 102.1(4) . . ?
C2 Co2 Co1 52.2(3) . . ?
C1 Co2 Co1 50.6(3) . . ?
P2 Co2 Co1 153.40(12) . . y
O21 C21 Co2 178.9(12) . . ?
O22 C22 Co2 174.2(10) . . ?
O23B P2 O25B 118.1(12) . . ?
O23B P2 O24 76.0(13) . . ?
O25B P2 O24 92.1(10) . . ?
O23B P2 O23A 39.8(11) . . ?
O25B P2 O23A 103.1(10) . . ?
O24 P2 O23A 113.5(7) . . ?
O23B P2 O25A 107.6(14) . . ?
O25B P2 O25A 32.0(8) . . ?
O24 P2 O25A 120.2(10) . . ?
O23A P2 O25A 77.7(11) . . ?
O23B P2 Co2 124.4(10) . . ?
O25B P2 Co2 116.9(6) . . ?
O24 P2 Co2 109.0(5) . . ?
O23A P2 Co2 119.0(5) . . ?
O25A P2 Co2 114.8(7) . . ?
C23 O23A P2 117.4(12) . . ?
P2 O23B C23 121(2) . . ?
O23A C23 O23B 41.2(10) . . ?
C24 O24 P2 135.2(15) . . ?
C25A O25A P2 159(3) . . ?
C25B O25B P2 115.8(15) . . ?
C2 C1 C16 142.1(9) . . y
C2 C1 Co1 71.6(6) . . ?
C16 C1 Co1 140.7(8) . . ?
C2 C1 Co2 68.5(5) . . ?
C16 C1 Co2 126.8(6) . . ?
Co1 C1 Co2 77.0(4) . . ?
C1 C2 C28 143.0(9) . . y
C1 C2 Co2 71.4(5) . . ?
C28 C2 Co2 137.3(7) . . ?
C1 C2 Co1 68.1(6) . . ?
C28 C2 Co1 130.9(6) . . ?
Co2 C2 Co1 76.8(3) . . ?
C111 C16 C17 116.0(10) . . ?
C111 C16 C1 121.9(10) . . ?
C17 C16 C1 122.0(10) . . ?
C18 C17 C16 121.6(11) . . ?
C17 C18 C19 121.0(12) . . ?
C110 C19 C18 118.6(12) . . ?
C19 C110 C111 120.7(12) . . ?
C110 C111 C16 121.9(11) . . ?
C210 C26 C27 120.2(10) 5_656 . ?
C27 C28 C2 116.2(8) . . y
C27 C28 C29 120.6(8) . . y
C28 C27 C26 119.9(9) . . y
C29 C28 C2 123.3(9) . . y
C210 C29 C28 122.9(8) . . y
C210 C29 C29 118.5(11) . 5_656 y
C28 C29 C29 118.6(11) . 5_656 y
C26 C210 C29 122.2(8) 5_656 . y
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
Co1 Co2 2.4368(19) . y
Co1 C1 1.934(10) . y
Co1 C2 1.978(9) . y
Co1 P1 2.135(3) . y
P1 O13 1.582(6) . y
P1 O15 1.582(7) . y
P1 O14 1.621(6) . y
Co1 C11 1.757(14) . y
C11 O11 1.181(12) . y
Co1 C12 1.743(10) . y
C12 O12 1.180(10) . y
O13 C13 1.415(11) . ?
O14 C14 1.445(10) . ?
O15 C15 1.436(10) . ?
Co2 C1 1.982(9) . y
Co2 C2 1.945(7) . y
Co2 C21 1.741(10) . y
C21 O21 1.189(11) . y
Co2 C22 1.759(14) . y
C22 O22 1.178(13) . y
Co2 P2 2.131(3) . y
P2 O23A 1.622(16) . y
P2 O23B 1.47(2) . ?
P2 O24 1.600(13) . y
P2 O25B 1.601(17) . y
P2 O25A 1.66(2) . y
O23A C23 1.451(18) . ?
O23B C23 1.55(3) . ?
O24 C24 1.234(16) . ?
O25A C25A 1.07(3) . ?
O25B C25B 1.58(3) . ?
C1 C2 1.346(11) . y
C1 C16 1.476(13) . y
C2 C28 1.495(11) . y
C16 C111 1.397(13) . ?
C16 C17 1.421(13) . ?
C17 C18 1.372(14) . ?
C18 C19 1.388(16) . ?
C19 C110 1.382(14) . ?
C110 C111 1.388(14) . ?
C26 C27 1.411(11) . y
C26 C210 1.361(11) 5_656 y
C27 C28 1.380(12) . y
C28 C29 1.419(12) . y
C29 C210 1.391(12) . y
C29 C29 1.441(15) 5_656 y
C210 C26 1.361(11) 5_656 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
P1 Co1 Co2 P2 3.5(4)
C16 C1 C2 C28 25(2)
