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_7028578
_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                   13.6906(4)
_cell_length_b                   12.6908(9)
_cell_length_c                   10.8131(9)
_cell_measurement_pressure       820000(40000)
_cell_measurement_reflns_used    3510
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3898
_cell_measurement_theta_min      1.4844
_cell_volume                     1878.7(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         820000(40000)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.539
_diffrn_measured_fraction_theta_max 0.466
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0002353000
_diffrn_orient_matrix_UB_12      -0.0370750000
_diffrn_orient_matrix_UB_13      -0.0490885000
_diffrn_orient_matrix_UB_21      -0.0086161000
_diffrn_orient_matrix_UB_22      0.0412228000
_diffrn_orient_matrix_UB_23      -0.0429487000
_diffrn_orient_matrix_UB_31      0.0510746000
_diffrn_orient_matrix_UB_32      0.0071306000
_diffrn_orient_matrix_UB_33      -0.0070219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.539
_diffrn_reflns_Laue_measured_fraction_max 0.466
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11178
_diffrn_reflns_point_group_measured_fraction_full 0.542
_diffrn_reflns_point_group_measured_fraction_max 0.457
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.452
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91653
_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    1.781
_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         0.418
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2169
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0365P)^2^+2.0987P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.545
_reflns_Friedel_fraction_max     0.446
_reflns_number_gt                1584
_reflns_number_total             2169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52035h.txt
_cod_data_source_block           d2a
_cod_database_code               7028578
_chemical_oxdiff_formula         'C40 H40 N12 Cl4 Co3'
_reflns_odcompleteness_completeness 50.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelx_hkl_checksum              29176
_shelxl_version_number           2013-2