Employing Dianionic Macrocyclic Tetracarbenes To Synthesize Neutral Divalent Metal Complexes
Bass, Heather M.; Cramer, S. Alan; McCullough, Alexander S.; Bernstein, Karl J.; Murdock, Christopher R.; Jenkins, David M.; Organometallics 32 (2013) 2160–; doi:10.1021/om400043z

data_4080506
_publ_section_title
;
 Employing Dianionic Macrocyclic Tetracarbenes To Synthesize Neutral
 Divalent Metal Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2160
_journal_paper_doi               10.1021/om400043z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C26 H48 B2 I2 N8 O2 S2'
_chemical_formula_weight         844.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.930(2)
_cell_angle_beta                 95.430(2)
_cell_angle_gamma                97.572(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5435(5)
_cell_length_b                   8.6724(5)
_cell_length_c                   12.6108(8)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.71
_cell_volume                     913.63(10)
_computing_molecular_graphics    'Diamond 3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18879
_diffrn_reflns_theta_full        30.59
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.870
_exptl_absorpt_correction_T_max  0.799
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.511
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         5444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0401P)^2^+0.4400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                5230
_reflns_number_total             5444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400043z_si_002.cif
_cod_data_source_block           macroI2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        913.63(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080506