A structural study of a three-membered linear metal chain compound at elevated pressure.
Madsen, Solveig R.; Thomsen, Maja K.; Scheins, Stephan; Chen, Yu-Sheng; Finkelmeier, Nils; Stalke, Dietmar; Overgaard, Jacob; Iversen, Bo B.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1313–1320; doi:10.1039/c3dt52035h

data_7028577
_publ_section_title
;
 A structural study of a three-membered linear metal chain compound at
 elevated pressure.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1313
_journal_page_last               1320
_journal_paper_doi               10.1039/c3dt52035h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C40 H32 Cl2 Co3 N12, C H2 Cl2'
_chemical_formula_sum            'C41 H34 Cl4 Co3 N12'
_chemical_formula_weight         1013.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-05-22
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr  9 2013 14:10:59, GUI svn.r4458)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8547(4)
_cell_length_b                   12.7941(9)
_cell_length_c                   11.0243(9)
_cell_measurement_pressure       320000(30000)
_cell_measurement_reflns_used    5268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5354
_cell_measurement_theta_min      1.4668
_cell_volume                     1954.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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
;
_diffrn_ambient_pressure         320000(30000)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.571
_diffrn_measured_fraction_theta_max 0.498
_diffrn_measurement_details
;
  1 omega   -6.00   49.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774  -39.0000 -167.0000 55

  2 omega   94.00  119.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774    0.0000  -90.0000 25

  3 omega  -26.00    2.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774   39.0000  -12.0000 28

  4 omega    3.00   30.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774   81.0000  151.0000 27

  5 omega   46.00   72.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774 -114.0000 -135.0000 26

  6 omega  -32.00   -7.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774   97.0000  -35.0000 25

  7 omega  -49.00  -23.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586   57.0000  150.0000 26

  8 omega   55.00   80.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586  178.0000  -60.0000 25

  9 omega  -56.00  -30.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586   97.0000  143.0000 26

 10 omega  -19.00    7.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586   19.0000  -30.0000 26

 11 omega  -36.00   -2.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586   53.0000  162.0000 34

 12 omega  -18.00   16.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586  -53.0000   17.0000 34

 13 omega    9.00   35.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586 -114.0000   45.0000 26

 14 omega  -40.00   -8.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774  114.0000  -45.0000 32

 15 omega  -23.00   64.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774  -39.0000   12.0000 87

 16 omega  -53.00   -8.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774  135.0000  123.0000 45

 17 omega  -24.00   26.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586  -39.0000 -167.0000 50

 18 omega  -64.00    8.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586   81.0000  151.0000 72

 19 omega  -23.00   26.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586  -39.0000   12.0000 49

 20 omega  -64.00  -39.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586   81.0000  -29.0000 25

 21 omega    3.00   31.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586  -99.0000   30.0000 28

 22 omega  -92.00   -8.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5586  135.0000  -57.0000 84

 23 omega   -6.00   49.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7774  -39.0000 -167.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0002307000
_diffrn_orient_matrix_UB_12      0.0370090000
_diffrn_orient_matrix_UB_13      -0.0479780000
_diffrn_orient_matrix_UB_21      0.0085459000
_diffrn_orient_matrix_UB_22      -0.0406884000
_diffrn_orient_matrix_UB_23      -0.0423245000
_diffrn_orient_matrix_UB_31      -0.0504536000
_diffrn_orient_matrix_UB_32      -0.0070648000
_diffrn_orient_matrix_UB_33      -0.0069243000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.571
_diffrn_reflns_Laue_measured_fraction_max 0.498
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20518
_diffrn_reflns_point_group_measured_fraction_full 0.579
_diffrn_reflns_point_group_measured_fraction_max 0.494
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.598
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 716 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0003(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+3.7012P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.589
_reflns_Friedel_fraction_max     0.490
_reflns_number_gt                1774
_reflns_number_total             2470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52035h.txt
_cod_data_source_block           d1a
_cod_database_code               7028577
_chemical_oxdiff_formula         'C40 H40 N12 Cl4 Co3'
_reflns_odcompleteness_completeness 53.82
_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
2. Restrained distances
 C21A-Cl3A = C21A-Cl2A
 1.7 with sigma of 0.5
 Cl2A-Cl3A
 2.95 with sigma of 0.5
 C21B-Cl3B = C21B-Cl2B
 1.7 with sigma of 0.5
 Cl2B-Cl3B
 2.95 with sigma of 0.8
3. Restrained planarity
 N1, C1, C2, C3, C4, C5
 with sigma of 0.1
 N2, C6, C7, C8, C9, C10
 with sigma of 0.1
 N3, C11, C12, C13, C14, C15
 with sigma of 0.1
 N4, C16, C17, C18, C19, C20
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C21A \\sim C21B \\sim Cl2A \\sim Cl2B \\sim Cl3A \\sim Cl3B: within 5A with sigma of 0.02 and sigma for terminal atoms of 0.03
5. Same fragment restrains
{N1, C5, C4, C3, C2, C1}
as
{N1, C1, C2, C3, C4, C5}
{C21B, Cl2B, Cl3B}
as
{C21A, Cl2A, Cl3A}
6. Others
 0.5*Sof(C21A)=0.5*Sof(H21A)=0.5*Sof(H21B)=0.5*Sof(Cl2A)=0.5*Sof(Cl3A)=1-0.5*
 Sof(C21B)=1-0.5*Sof(H21C)=1-0.5*Sof(H21D)=1-0.5*Sof(Cl2B)=1-0.5*Sof(Cl3B)
7.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C21B(H21C,H21D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_hkl_checksum              80746
_shelxl_version_number           2013-2