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_7019282
_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
'C40 H32 N12 Cr2 Mn, 2(S O3 C F3), 0.65(C H2 Cl2)'
_chemical_formula_sum            'C42.65 H33.3 Cl1.3 Cr2 F6 Mn N12 O6 S2'
_chemical_formula_weight         1193.06
_chemical_name_common            Cr2Mn(dpa)4(OTf)2(CH2Cl2)0.65
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                90.00
_cell_angle_beta                 108.1440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.4980(8)
_cell_length_b                   17.8985(4)
_cell_length_c                   16.8592(4)
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3381
_cell_measurement_theta_min      2.5426
_cell_volume                     9892.3(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            108760
_diffrn_reflns_theta_full        26.78
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.8929
_exptl_absorpt_correction_T_min  0.8204
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2007)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4818
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1317
_refine_ls_number_reflns         19453
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+80.6260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                17589
_reflns_number_total             19453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30150d.txt
_cod_data_source_block           compound2(100K)
_cod_original_sg_symbol_H-M      Cc
_cod_original_formula_sum        'C42.65 H33.30 Cl1.30 Cr2 F6 Mn N12 O6 S2'
_cod_database_code               7019282