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_7028575
_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                   13.502(2)
_cell_length_b                   12.5615(13)
_cell_length_c                   10.381(4)
_cell_measurement_pressure       2170000(50000)
_cell_measurement_reflns_used    2009
_cell_measurement_temperature    292.4(6)
_cell_measurement_theta_max      25.6446
_cell_measurement_theta_min      1.5051
_cell_volume                     1760.7(7)
_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         2170000(50000)
_diffrn_ambient_temperature      292.4(6)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.519
_diffrn_measured_fraction_theta_max 0.499
_diffrn_measurement_details
;
  1 omega   -1.00   36.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       12.6171  -39.0000 -167.0000 37

  2 omega   14.00   40.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4764 -135.0000 -123.0000 26

  3 omega  -52.00  -22.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4764   57.0000  150.0000 30

  4 omega   -6.00   21.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4764   57.0000  150.0000 27

  5 omega    2.00   30.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4764  -67.0000   23.0000 28

  6 omega  -46.00    7.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       12.6171  114.0000  -45.0000 53

  7 omega   16.00   85.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       12.6171 -135.0000   57.0000 69

  8 omega -114.00  -49.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4764    0.0000  -90.0000 65

  9 omega   -2.00   37.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.4764  -99.0000   30.0000 39
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0293319000
_diffrn_orient_matrix_UB_12      0.0022245000
_diffrn_orient_matrix_UB_13      0.0566494000
_diffrn_orient_matrix_UB_21      0.0361945000
_diffrn_orient_matrix_UB_22      -0.0327151000
_diffrn_orient_matrix_UB_23      -0.0298098000
_diffrn_orient_matrix_UB_31      0.0242901000
_diffrn_orient_matrix_UB_32      0.0459498000
_diffrn_orient_matrix_UB_33      -0.0239227000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1257
_diffrn_reflns_Laue_measured_fraction_full 0.519
_diffrn_reflns_Laue_measured_fraction_max 0.499
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4005
_diffrn_reflns_point_group_measured_fraction_full 0.465
_diffrn_reflns_point_group_measured_fraction_max 0.445
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.700
_diffrn_reflns_theta_min         2.214
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42054
_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    1.900
_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         0.617
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 295 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     589
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1256P)^2^+4.3791P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2406
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_full    0.404
_reflns_Friedel_fraction_max     0.385
_reflns_number_gt                997
_reflns_number_total             1496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52035h.txt
_cod_data_source_block           c3a
_cod_database_code               7028575
_chemical_oxdiff_formula         'C40 H40 N12 Cl4 Co3'
_reflns_odcompleteness_completeness 58.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_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
 1.77 with sigma of 0.08
 Cl2A-Cl3A
 2.95 with sigma of 0.1
 C21B-Cl3B = C21B-Cl2B
 1.77 with sigma of 0.08
 Cl2B-Cl3B
 2.95 with sigma of 0.1
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
Cl3A \\sim C21A \\sim Cl3B \\sim C21B \\sim Cl2A \\sim Cl2B: within 4A 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              45362
_shelxl_version_number           2013-2