Element misidentification in X-ray crystallography: a reassessment of the [MCl2(diazadiene)] (M = Cr, Mo, W) series.
Greene, Angelique F.; Chandrasekaran, P.; Yan, Yong; Mague, Joel T.; Donahue, James P.; Inorganic chemistry 53 (2014) 308–317; doi:10.1021/ic402246d

data_4337539
_publ_section_title
;
 Element misidentification in X-ray crystallography: a reassessment of the
 [MCl2(diazadiene)] (M = Cr, Mo, W) series.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              308
_journal_page_last               317
_journal_paper_doi               10.1021/ic402246d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C23 H30 Br2 Cl2 N2 Zn'
_chemical_formula_weight         630.58
_chemical_name_systematic
; 
 ? 
;
_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                 90.002(30)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.625(3)
_cell_length_b                   14.625(3)
_cell_length_c                   14.336(3)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.774
_cell_measurement_theta_min      2.5615
_cell_volume                     2647.0(10)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS, 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.701
_diffrn_measured_fraction_theta_max 0.754
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29645
_diffrn_reflns_theta_full        27.83
_diffrn_reflns_theta_max         27.83
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    4.162
_exptl_absorpt_correction_T_max  0.6762
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.926
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                3544
_reflns_number_total             4742
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic402246d_si_003.cif
_cod_data_source_block           jpd535a
_cod_original_cell_volume        2646.9(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4337539