Structural classification of metal complexes with three-coordinate centres.
Davis, Timothy L.; Watts, Joshua L.; Brown, Kenneth J.; Hewage, Jeewantha S.; Treleven, Alexander R.; Lindeman, Sergey V.; Gardinier, James R.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15408–15412; doi:10.1039/c5dt02773j

data_7036056
_publ_section_title
;
 Structural classification of metal complexes with three-coordinate
 centres.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15408
_journal_page_last               15412
_journal_paper_doi               10.1039/c5dt02773j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'F6 Sb, C23 H18 Ag Fe N4, 0.5(C H2 Cl2), C H4 O'
_chemical_formula_sum            'C24.5 H23 Ag Cl F6 Fe N4 O Sb'
_chemical_formula_weight         824.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2015-05-13 deposited with the CCDC.
2015-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                66.887(3)
_cell_angle_beta                 85.557(3)
_cell_angle_gamma                67.084(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4401(3)
_cell_length_b                   11.0107(4)
_cell_length_c                   13.8825(4)
_cell_measurement_reflns_used    12812
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.7410
_cell_measurement_theta_min      3.5910
_cell_volume                     1346.54(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 16.1500
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.8928
_diffrn_measurement_details
;
  1 omega  -48.00   31.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -57.0000    0.0000 79

  2 omega   -6.00   88.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909   77.0000  150.0000 94

  3 omega   16.00   57.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -99.0000   60.0000 41

  4 omega   33.00   59.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -99.0000  -60.0000 26

  5 omega  -55.00   57.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -19.0000 -150.0000 112

  6 omega   69.00   95.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909 -178.0000  -30.0000 26

  7 omega   35.00   94.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  178.0000 -120.0000 59

  8 omega   -3.00   87.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000  -90.0000 90

  9 omega   -3.00   87.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000   90.0000 90

 10 omega   35.00   94.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  178.0000  -30.0000 59

 11 omega   -3.00   87.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000    0.0000 90

 12 omega   -3.00   22.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909   57.0000  150.0000 25

 13 omega  -20.00   60.00   1.0000    3.8100
omega____ theta____ kappa____ phi______ frames
    -       18.0909  -99.0000  120.0000 80
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0273366000
_diffrn_orient_matrix_UB_12      -0.0754041000
_diffrn_orient_matrix_UB_13      0.0149896000
_diffrn_orient_matrix_UB_21      0.0375386000
_diffrn_orient_matrix_UB_22      -0.0096759000
_diffrn_orient_matrix_UB_23      0.0446899000
_diffrn_orient_matrix_UB_31      -0.0576867000
_diffrn_orient_matrix_UB_32      -0.0037760000
_diffrn_orient_matrix_UB_33      0.0298127000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24078
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.1821
_exptl_crystal_size_mid          0.0821
_exptl_crystal_size_min          0.0538
_refine_diff_density_max         0.813
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0291
_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/[\s^2^(Fo^2^)+(0.0260P)^2^+2.2591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                5645
_reflns_number_total             6494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02773j3.cif
_cod_data_source_block           2_acetone_pt5dcm
_cod_depositor_comments
'Adding full bibliography for 7036055--7036056.cif.'
_cod_original_cell_volume        1346.54(8)
_cod_original_formula_sum        'C24.50 H23 Ag Cl F6 Fe N4 O Sb'
_cod_database_code               7036056
_chemical_oxdiff_formula         'Fe C23 H18 N4 Ag Sb F6 C H4 O (C H2 Cl2)0.5'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23)
3.c Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
3.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;