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_7028576
_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   mixed
_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                   13.3971(13)
_cell_length_b                   12.4500(6)
_cell_length_c                   10.192(2)
_cell_measurement_pressure       3200000(100000)
_cell_measurement_reflns_used    1621
_cell_measurement_temperature    292.57(10)
_cell_measurement_theta_max      28.3829
_cell_measurement_theta_min      1.6323
_cell_volume                     1700.0(4)
_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         3200000(100000)
_diffrn_ambient_temperature      292.57(10)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.556
_diffrn_measured_fraction_theta_max 0.476
_diffrn_measurement_details
;
  1 omega   65.00  106.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9119  178.0000  -90.0000 41

  2 omega   21.00   54.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9119  -39.0000   12.0000 33

  3 omega  -17.00   29.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9119  -19.0000 -180.0000 46

  4 omega  -47.00  -17.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9119  135.0000  -57.0000 30

  5 omega  -81.00  -49.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9119    0.0000  -90.0000 32

  6 omega  -25.00   13.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9119   81.0000  151.0000 38

  7 omega   -6.00   31.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931  -97.0000 -143.0000 37

  8 omega  -29.00   -4.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931  -39.0000 -167.0000 25

  9 omega  -79.00    7.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6931  114.0000  -45.0000 86
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0302831000
_diffrn_orient_matrix_UB_12      0.0016119000
_diffrn_orient_matrix_UB_13      0.0575296000
_diffrn_orient_matrix_UB_21      0.0358430000
_diffrn_orient_matrix_UB_22      -0.0330393000
_diffrn_orient_matrix_UB_23      -0.0311575000
_diffrn_orient_matrix_UB_31      0.0245370000
_diffrn_orient_matrix_UB_32      0.0461879000
_diffrn_orient_matrix_UB_33      -0.0242746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.1249
_diffrn_reflns_Laue_measured_fraction_full 0.556
_diffrn_reflns_Laue_measured_fraction_max 0.476
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5186
_diffrn_reflns_point_group_measured_fraction_full 0.527
_diffrn_reflns_point_group_measured_fraction_max 0.436
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.445
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72425
_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    1.980
_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         0.527
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 360 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.001(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         1870
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+1.7852P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1983
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.494
_reflns_Friedel_fraction_max     0.390
_reflns_number_gt                1112
_reflns_number_total             1870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52035h.txt
_cod_data_source_block           c4a
_cod_database_code               7028576
_chemical_oxdiff_formula         'C40 H40 N12 Cl4 Co3'
_reflns_odcompleteness_completeness 52.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 Cl2A-C21A
 1.7 with sigma of 0.09
 C21A-Cl3A
 1.7 with sigma of 0.09
 Cl3B-C21B
 1.7 with sigma of 0.09
 C21B-Cl2B
 1.7 with sigma of 0.09
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 Cl3A \\sim Cl2B \\sim Cl3B: within 5A with sigma of 0.03 and sigma for terminal atoms of 0.05
5. Others
 1-0.5*Sof(C21B)=1-0.5*Sof(H21A)=1-0.5*Sof(H21B)=0.5*Sof(Cl2A)=0.5*Sof(Cl3A)=
 0.5*Sof(C21A)=0.5*Sof(H21C)=0.5*Sof(H21D)=1-0.5*Sof(Cl2B)=1-0.5*Sof(Cl3B)
 Fixed Uiso: H2(0.05) H3(0.053) H4(0.067) H5(0.045) H7(0.042) H8(0.043)
 H9(0.061) H10(0.033) H11(0.048) H12(0.065) H13(0.052) H14(0.047) H16(0.07)
 H17(0.068) H18(0.072) H19(0.049)
 Fixed X: H2(0.365901) H3(0.443) H4(0.5709) H5(0.6355) H7(0.263901)
 H8(0.242399) H9(0.3655) H10(0.501901) H11(0.8041) H12(0.9382) H13(0.9084)
 H14(0.751901) H16(0.6505) H17(0.701) H18(0.6946) H19(0.6447) Co2(0.5)
 Fixed Y: H2(0.603201) H3(0.723101) H4(0.8265) H5(0.7876) H7(0.6725)
 H8(0.853901) H9(0.9575) H10(0.874599) H11(0.657301) H12(0.5585) H13(0.413301)
 H14(0.365301) H16(0.7627) H17(0.718) H18(0.544399) H19(0.4127) Co2(0.5)
 Fixed Z: H2(-0.380099) H3(-0.5169) H4(-0.4336) H5(-0.234099) H7(0.222301)
 H8(0.2042) H9(0.110901) H10(0.021601) H11(0.0262) H12(-0.0446) H13(-0.176299)
 H14(-0.236) H16(0.2415) H17(0.4452) H18(0.517) H19(0.3718)
6.a Secondary CH2 refined with riding coordinates:
 C21B(H21A,H21B), C21A(H21C,H21D)
;
_shelx_hkl_checksum              17079
_shelxl_version_number           2013-2