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_7028574
_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                   13.7147(15)
_cell_length_b                   12.7050(6)
_cell_length_c                   10.8427(17)
_cell_measurement_pressure       740000(40000)
_cell_measurement_reflns_used    2180
_cell_measurement_temperature    293.0(9)
_cell_measurement_theta_max      28.4153
_cell_measurement_theta_min      1.5990
_cell_volume                     1889.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.1t (release 26-07-2012 CrysAlis171 .NET)
(compiled Aug  1 2012,17:32:42)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.1t (release 26-07-2012 CrysAlis171 .NET)
(compiled Aug  1 2012,17:32:42)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.1t (release 26-07-2012 CrysAlis171 .NET)
(compiled Aug  1 2012,17:32:42)
;
_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         740000(40000)
_diffrn_ambient_temperature      293.0(9)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.5537
_diffrn_measured_fraction_theta_max 0.7432
_diffrn_measurement_details
;
  1 omega  -21.00   31.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5994  -26.0000    7.0000 52

  2 omega  -14.00   12.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5994   46.0000  -11.0000 26

  3 omega   37.00   64.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5994  -99.0000   60.0000 27

  4 omega   68.00  106.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5994 -178.0000  -90.0000 38

  5 omega   -3.00   22.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5369 -114.0000 -135.0000 25

  6 omega  -32.00    6.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5994   97.0000  143.0000 38

  7 omega  -55.00   28.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5369   39.0000  -12.0000 83

  8 omega  -29.00   26.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5369  -39.0000 -167.0000 55

  9 omega    3.00   39.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.5369 -114.0000   45.0000 36
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0312663000
_diffrn_orient_matrix_UB_12      -0.0018054000
_diffrn_orient_matrix_UB_13      0.0520219000
_diffrn_orient_matrix_UB_21      -0.0343326000
_diffrn_orient_matrix_UB_22      0.0319421000
_diffrn_orient_matrix_UB_23      -0.0314746000
_diffrn_orient_matrix_UB_31      -0.0227299000
_diffrn_orient_matrix_UB_32      -0.0457279000
_diffrn_orient_matrix_UB_33      -0.0240484000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.1207
_diffrn_reflns_Laue_measured_fraction_full 0.584
_diffrn_reflns_Laue_measured_fraction_max 0.499
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7040
_diffrn_reflns_point_group_measured_fraction_full 0.571
_diffrn_reflns_point_group_measured_fraction_max 0.470
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.491
_diffrn_reflns_theta_min         2.185
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.1t (release 26-07-2012 CrysAlis171 .NET)
(compiled Aug  1 2012,17:32:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.1612
_exptl_crystal_size_mid          0.1166
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 475 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000(2)
_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         2255
_refine_ls_number_restraints     588
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0391P)^2^+2.6811P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    0.556
_reflns_Friedel_fraction_max     0.438
_reflns_number_gt                1432
_reflns_number_total             2255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52035h.txt
_cod_data_source_block           c2a
_cod_database_code               7028574
_chemical_oxdiff_formula         'Co3 Cl2 C40 N12 H40'
_reflns_odcompleteness_completeness 55.37
_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
 Cl2B-C21B
 1.79 with sigma of 0.05
 C21B-Cl3B
 1.79 with sigma of 0.05
 Cl2A-C21A
 1.79 with sigma of 0.05
 C21A-Cl3A
 1.79 with sigma of 0.05
 Cl3B-Cl2B
 2.9 with sigma of 0.2
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 Cl3B \\sim Cl3A \\sim Cl2B: within 5A with sigma of 0.03 and sigma for terminal atoms of 0.06
5. Same fragment restrains
{N2, C6, C7, C8, C9, C10}
{N3, C11, C12, C13, C14, C15}
{N4, C16, C17, C18, C19, C20}
{N1, C5, C4, C3, C2, C1}
{C1, C2, C3, C4, C5, N1}
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              43606
_shelxl_version_number           2013-2