A [I−Ca−I−Ca−I−Ca−I]2+Chain Stabilized by Two Chelating β-Diketiminate Ligands
Sarish, Sankaranarayana Pillai; Jana, Anukul; Roesky, Herbert W.; Schulz, Thomas; Stalke, Dietmar; Organometallics 29 (2010) 2901–; doi:10.1021/om100165s

data_4065860
_publ_section_title
;
 A [I&#x2212;Ca&#x2212;I&#x2212;Ca&#x2212;I&#x2212;Ca&#x2212;I]2+Chain
 Stabilized by Two Chelating \b-Diketiminate Ligands
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2901
_journal_paper_doi               10.1021/om100165s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C62 H102 Ca3 I4 N8'
_chemical_formula_weight         1587.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 116.273(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.550(6)
_cell_length_b                   16.668(6)
_cell_length_c                   14.904(5)
_cell_measurement_reflns_used    6998
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.44
_cell_volume                     3464(2)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2.2-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics    'XP in SHELXTL ver. 6.10'
_computing_publication_material  'XP in SHELXTL ver. 6.10'
_computing_structure_refinement  'SHELXL in SHELXTL ver. 6.10'
_computing_structure_solution    'SHELXS in SHELXTL ver. 6.10'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'INCOATEC Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            49063
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5823
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2007/5
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6112
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+17.3674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                4500
_reflns_number_total             6112
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100165s_si_001.cif
_cod_data_source_block           ss900
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4065860