Binding and activation of small molecules by a quintuply bonded chromium dimer
Jingmei Shen; Glenn P. A. Yap; Klaus H. Theopold; Chem.Commun. 50 (2014) 2579–; doi:10.1039/c3cc48746f

data_7111923
_publ_section_title
;
 Binding and activation of small molecules by a quintuply bonded chromium
 dimer
;
_journal_name_full               Chem.Commun.
_journal_page_first              2579
_journal_paper_doi               10.1039/c3cc48746f
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C82 H102 Cr2 N4 O3'
_chemical_formula_weight         1295.67
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.757(6)
_cell_angle_beta                 100.752(5)
_cell_angle_gamma                97.594(6)
_cell_formula_units_Z            2
_cell_length_a                   12.257(4)
_cell_length_b                   13.447(4)
_cell_length_c                   22.146(7)
_cell_measurement_reflns_used    628
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.17
_cell_measurement_theta_min      2.22
_cell_volume                     3551.9(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1652
_diffrn_reflns_av_unetI/netI     0.3188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48405
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.368
_diffrn_reflns_theta_min         1.762
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.117
_platon_squeeze_details
; 

Void space analysis consistent with initial solutions showing one 
severely disordered diethylether solvent molecule in the asymmetric 
unit (i.e. two in the unit cell) near an inversion center.

PLATON Reference : 
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
Spek, A.L. (2009). Acta Cryst. D65, 148-155.

;
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         17665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.2342
_refine_ls_R_factor_gt           0.0831
_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^)+(0.0029P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5165
_reflns_number_total             17665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc48746f.txt
_cod_data_source_block           klat854s-sr
_cod_original_cell_volume        3551.9(18)
_cod_database_code               7111923
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2013-2
_shelx_res_checksum              78704
_shelx_hkl_checksum              97051