Synthesis, characterization and thermal properties of trimetallic N(3)-Cr[quadruple bond, length as m-dash]CrM-N(3) azide complexes with M = Cr, Mn, Fe, and Co.
Turov, Yevgeniya; Berry, John F.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 8153–8161; doi:10.1039/c2dt30150d

data_7019283
_publ_section_title
;
 Synthesis, characterization and thermal properties of trimetallic
 N(3)-Cr[quadruple bond, length as m-dash]CrM-N(3) azide complexes with M
 = Cr, Mn, Fe, and Co.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8153
_journal_page_last               8161
_journal_paper_doi               10.1039/c2dt30150d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'Cr2 Mn C40 H32 N18'
_chemical_formula_sum            'C40 H32 Cr2 Mn N18'
_chemical_formula_weight         923.78
_chemical_name_common            Cr2Mn(dpa)4(N3)2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.002(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.8889(7)
_cell_length_b                   16.5572(8)
_cell_length_c                   17.0566(8)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2673
_cell_measurement_theta_min      2.3450
_cell_volume                     3900.9(3)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60040
_diffrn_reflns_theta_full        25.54
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7634
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2007)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+7.8024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                5822
_reflns_number_total             7218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30150d.txt
_cod_data_source_block           compound4(100K)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7019283