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_7019284
_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 Cr2 Fe N18, C4 H10 O'
_chemical_formula_sum            'C44 H42 Cr2 Fe N18 O'
_chemical_formula_weight         998.11
_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                90.00
_cell_angle_beta                 104.433(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9450(5)
_cell_length_b                   16.2777(5)
_cell_length_c                   17.6430(6)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0977
_cell_measurement_theta_min      2.3473
_cell_volume                     4434.7(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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         'microfocus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            121446
_diffrn_reflns_theta_full        30.13
_diffrn_reflns_theta_max         30.13
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.9091
_exptl_absorpt_correction_T_min  0.7776
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2007)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2055
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         13042
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0403
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1513
_reflns_number_gt                10839
_reflns_number_total             13042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30150d.txt
_cod_data_source_block           compound5(100K)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7019284