ansa-Calcocenes: <i>rac</i>-[bis(3,3'-biacenaphthylenido)]bis(tetrahydrofuran)calcium
Sinnema, Piet-Jan; Twamley, Brendan; Shapiro, Pamela J.; Acta Crystallographica Section E 57 (2001) m438–m440; doi:10.1107/S1600536801014751

data_2200736
_publ_section_title
;
 ansa-Calcocenes:
 <i>rac</i>-[bis(3,3'-biacenaphthylenido)]bis(tetrahydrofuran)calcium
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m438
_journal_page_last               m440
_journal_paper_doi               10.1107/S1600536801014751
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Ca(C24 H12) (C4 H8 O)2]'
_chemical_formula_moiety         'C32 H32 Ca O2'
_chemical_formula_sum            'C32 H32 Ca O2'
_chemical_formula_weight         488.66
_chemical_name_common            (acenaphtylenide)2Ca.2THF
_chemical_name_systematic
;
rac-[bis(3,3'-biacenaphthylenido)]bis(tetrahydrofuran-O)calcium
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1497(14)
_cell_length_b                   8.6805(7)
_cell_length_c                   35.047(3)
_cell_measurement_reflns_used    928
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.3
_cell_volume                     4913.2(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  'XCIF in SHELXTL'
_computing_structure_refinement  'XL in SHELXTL'
_computing_structure_solution    'XS in SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      203(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART 1K'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0744
_diffrn_reflns_av_sigmaI/netI    .0752
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            36582
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.2
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .28
_exptl_absorpt_correction_T_max  .986
_exptl_absorpt_correction_T_min  .935
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .05
_refine_diff_density_max         .78
_refine_diff_density_min         -.22
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .11(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8481
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          .091
_refine_ls_R_factor_gt           .054
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .128
_reflns_number_gt                5906
_reflns_number_total             8481
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6048.cif
_cod_data_source_block           I
_cod_database_code               2200736
_cod_database_fobs_code          2200736