Synthesis and unprecedented coordination behaviour of a novel 1,2,3-triphosphaferrocene complex.
Deng, Shining; Schwarzmaier, Christoph; Eichhorn, Christiane; Scherer, Otto; Wolmershäuser, Gotthelf; Zabel, Manfred; Scheer, Manfred; Chemical communications (Cambridge, England)  (2008) 4064–4066; doi:10.1039/b807658h

data_7103322
_publ_section_title
;
 Synthesis and unprecedented coordination behaviour of a novel
 1,2,3-triphosphaferrocene complex.
;
_journal_issue                   34
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4064
_journal_page_last               4066
_journal_paper_doi               10.1039/b807658h
_journal_year                    2008
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C54 H76 Br4 Cu4 Fe2 N2 P6, 1.5(C H2 Cl2)'
_chemical_formula_structural     'C54 H76 Br4 Cu4 Fe2 N2 P6, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C55.5 H79 Br4 Cl3 Cu4 Fe2 N2 P6'
_chemical_formula_weight         1751.88
_chemical_name_systematic        ?
_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
_cell_angle_alpha                110.545(7)
_cell_angle_beta                 94.432(6)
_cell_angle_gamma                104.171(6)
_cell_formula_units_Z            2
_cell_length_a                   15.1002(10)
_cell_length_b                   15.5709(11)
_cell_length_c                   16.3950(12)
_cell_measurement_reflns_used    11859
_cell_measurement_temperature    123
_cell_measurement_theta_max      62.7798
_cell_measurement_theta_min      3.0603
_cell_volume                     3442.8(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
1 phi -180.00 -120.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -1.3492 0.0000 - 0.0000 0.0000 60

2 omega -79.00 -24.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -1.3492 -75.0000 240.0000 0.0000 0.0000 55

3 omega -29.00 22.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -1.3492 45.0000 240.0000 0.0000 0.0000 51

4 omega 27.00 78.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 3.0060 45.0000 0.0000 0.0000 0.0000 51

5 omega -22.00 26.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 3.0060 45.0000 120.0000 0.0000 0.0000 48

6 omega -24.00 26.00 1.0000 50.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 3.0060 45.0000 0.0000 0.0000 0.0000 50

7 omega -60.00 -9.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 45.0000 120.0000 0.0000 0.0000 51

8 omega -106.00 -51.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -75.0000 0.0000 0.0000 0.0000 55

9 omega -159.00 -108.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -47.0000 322.0000 0.0000 0.0000 51

10 omega -106.00 -54.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -62.0000 51.0000 0.0000 0.0000 52

11 omega -118.00 -65.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 117.0000 233.0000 0.0000 0.0000 53

12 omega -162.00 -107.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -75.0000 240.0000 0.0000 0.0000 55

13 omega -158.00 -106.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -59.0000 77.0000 0.0000 0.0000 52

14 omega -118.00 -65.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 117.0000 50.0000 0.0000 0.0000 53

15 omega -112.00 -61.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 45.0000 240.0000 0.0000 0.0000 51

16 omega -158.00 -108.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -45.0000 0.0000 0.0000 0.0000 50

17 omega -60.00 -15.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 45.0000 0.0000 0.0000 0.0000 45

18 omega -112.00 -61.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 45.0000 0.0000 0.0000 0.0000 51

19 omega -105.00 -55.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -84.2355 -57.0000 182.0000 0.0000 0.0000 50

20 omega 12.00 63.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 -75.0000 240.0000 0.0000 0.0000 51

21 omega 55.00 84.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 63.0000 171.0000 0.0000 0.0000 29

22 omega 24.00 63.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 -75.0000 120.0000 0.0000 0.0000 39

23 omega 108.00 160.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 62.0000 78.0000 0.0000 0.0000 52

24 omega 72.00 119.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 -75.0000 240.0000 0.0000 0.0000 47

25 omega 11.00 39.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 -116.0000 93.0000 0.0000 0.0000 28

26 omega 52.00 92.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 -116.0000 93.0000 0.0000 0.0000 40

27 omega 64.00 98.00 1.0000 85.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 85.8923 -75.0000 120.0000 0.0000 0.0000 34

;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25040
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        62.95
_diffrn_reflns_theta_max         62.95
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.019
_exptl_absorpt_correction_T_max  1.07613
_exptl_absorpt_correction_T_min  0.89630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelike
_exptl_crystal_F_000             1750
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         10799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.2447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                8052
_reflns_number_total             10799
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b807658h.txt
_cod_data_source_block           ds210
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C55.50 H79 Br4 Cl3 Cu4 Fe2 N2 P6'
_cod_database_code               7103322