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_7028573
_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                   14.0472(12)
_cell_length_b                   12.9062(14)
_cell_length_c                   11.2407(5)
_cell_measurement_pressure       0.0(0)
_cell_measurement_reflns_used    2491
_cell_measurement_temperature    293.4(9)
_cell_measurement_theta_max      28.4724
_cell_measurement_theta_min      1.8080
_cell_volume                     2037.9(3)
_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
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_pressure         0.0(0)
_diffrn_ambient_temperature      293.4(9)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.584
_diffrn_measured_fraction_theta_max 0.500
_diffrn_measurement_details
;
  1 omega  -31.00   -4.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7556  114.0000  135.0000 27

  2 omega  -11.00   39.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7556  -57.0000 -150.0000 50

  3 omega  -34.00   -9.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931   53.0000  162.0000 25

  4 omega  -38.00   14.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931   26.0000   -7.0000 52

  5 omega   -1.00   27.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931  -97.0000   35.0000 28

  6 omega    4.00   78.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7556 -114.0000   45.0000 74

  7 omega  -32.00    5.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7556   97.0000  -35.0000 37

  8 omega  -38.00   44.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931   38.0000  150.0000 82

  9 omega  -13.00   24.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931  -81.0000   29.0000 37
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0338927000
_diffrn_orient_matrix_UB_12      0.0407277000
_diffrn_orient_matrix_UB_13      -0.0013760000
_diffrn_orient_matrix_UB_21      0.0237021000
_diffrn_orient_matrix_UB_22      -0.0245559000
_diffrn_orient_matrix_UB_23      -0.0480592000
_diffrn_orient_matrix_UB_31      -0.0289838000
_diffrn_orient_matrix_UB_32      0.0275229000
_diffrn_orient_matrix_UB_33      -0.0408681000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.584
_diffrn_reflns_Laue_measured_fraction_max 0.500
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8911
_diffrn_reflns_point_group_measured_fraction_full 0.575
_diffrn_reflns_point_group_measured_fraction_max 0.478
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.535
_diffrn_reflns_theta_min         2.143
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80087
_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    1.65
_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         0.440
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2480
_refine_ls_number_restraints     583
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0657P)^2^+0.3478P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.565
_reflns_Friedel_fraction_max     0.454
_reflns_number_gt                1449
_reflns_number_total             2480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52035h.txt
_cod_data_source_block           c1a
_cod_database_code               7028573
_chemical_oxdiff_formula         'Co3 Cl4 C42 N12 H40'
_reflns_odcompleteness_completeness 63.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     20.77
_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
 Cl3B-Cl2B
 2.9 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
C21A \\sim C21B \\sim Cl2A \\sim Cl3B \\sim Cl3A \\sim Cl2B: within 5A with sigma of 0.03 and sigma for terminal atoms of 0.03
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}
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              7445
_shelxl_version_number           2013-2