A low-temperature investigation of <i>trans</i>-diiodotetrakis(tetrahydrofuran)calcium(II)
Henderson, Kenneth W.; Rood, Jeffrey A.; Noll, Bruce C.; Acta Crystallographica Section E 61 (2005) m2006–m2007; doi:10.1107/S1600536805028254

data_2207072
_publ_section_title
;
 A low-temperature investigation of
 <i>trans</i>-diiodotetrakis(tetrahydrofuran)calcium(II)
;
_journal_coeditor_code           TK6253
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2006
_journal_page_last               m2007
_journal_paper_doi               10.1107/S1600536805028254
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Ca I2 (C8 H16 O2)2]'
_chemical_formula_moiety         'C16 H32 Ca I2 O4'
_chemical_formula_sum            'C16 H32 Ca I2 O4'
_chemical_formula_weight         582.30
_chemical_name_systematic
;
trans-diiodotetrakis(tetrahydrofuran)calcium(II)
;
_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                80.1560(10)
_cell_angle_beta                 89.4120(10)
_cell_angle_gamma                87.8770(10)
_cell_formula_units_Z            2
_cell_length_a                   8.442(2)
_cell_length_b                   9.858(2)
_cell_length_c                   13.610(3)
_cell_measurement_reflns_used    5033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.8
_cell_volume                     1115.2(4)
_computing_cell_refinement       'APEX2 and SAINT (Bruker--Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker--Nonius, 2004)'
_computing_data_reduction        'SAINT and SHELXTL (Sheldrick, 2004)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4361
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.282
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.146
_refine_diff_density_max         2.27
_refine_diff_density_min         -1.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         4361
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.058
_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^)+(0.1062P)^2^+6.8251P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.158
_refine_ls_wR_factor_ref         0.171
_reflns_number_gt                3852
_reflns_number_total             4361
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6253.cif
_cod_data_source_block           I
_cod_database_code               2207072
_cod_database_fobs_code          2207072