Synthesis and structure of η5-bonded pyrrolyl complexes of calcium and strontium
Schumann, Herbert; Gottfriedsen, Jochen; Demtschuk, Jörg; Chemical Communications  (1999) 2091–; doi:10.1039/a906654c

data_7110694
_publ_section_title
;
 Synthesis and structure of \h5-bonded pyrrolyl complexes of calcium and
 strontium
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2091
_journal_paper_doi               10.1039/a906654c
_journal_year                    1999
_chemical_formula_sum            'C45 H79 Ca1.5 N3 O1.5'
_chemical_formula_weight         746.23
_chemical_name_common            Di-tBu-pyrrolyl-THF-calcium
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 108.45(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.43(2)
_cell_length_b                   14.843(3)
_cell_length_c                   18.053(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      11.94
_cell_measurement_theta_min      6.54
_cell_volume                     9260(6)
_computing_cell_refinement       'CAD4/PC (Kretschmar, 1994)'
_computing_data_collection       'CAD4/PC (Kretschmar, 1994)'
_computing_data_reduction        'XCAD4 (Fr\"ohlich, 1994)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, Pritzkow, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7523
_diffrn_reflns_theta_full        23.89
_diffrn_reflns_theta_max         23.89
_diffrn_reflns_theta_min         1.18
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.225
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1686P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2314
_reflns_number_gt                4950
_reflns_number_total             7115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906654csup1.cif
_cod_data_source_block           jd37
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C45 H79 Ca1.50 N3 O1.50'
_cod_database_code               7110694