Alkali and Alkaline Earth Metal Complexes Ligated by an Ethynyl Substituted Cyclopentadienyl Ligand
Seifert, T.; Roesky, P.W.; Inorganics 5 (2017) 28–; doi:10.3390/inorganics5020028

data_1556493
_publ_section_title
;
 Alkali and Alkaline Earth Metal Complexes Ligated by an Ethynyl
 Substituted Cyclopentadienyl Ligand
;
_journal_name_full               Inorganics
_journal_page_first              28
_journal_paper_doi               10.3390/inorganics5020028
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C44 H74 Ca2 I2 O4 Si2'
_chemical_formula_sum            'C44 H74 Ca2 I2 O4 Si2'
_chemical_formula_weight         1057.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_cell_angle_alpha                90
_cell_angle_beta                 101.490(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4746(4)
_cell_length_b                   14.9924(8)
_cell_length_c                   21.7467(8)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    220
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      1.91
_cell_volume                     3027.1(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      220
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 100K'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14525
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.125
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.7284
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.276
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3630
_reflns_number_total             5910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           tps120-3h
_cod_database_code               1556493
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C20(H20A,H20B), C18(H18A,H18B), C22(H22A,
 H22B), C15(H15A,H15B), C17(H17A,H17B), C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              5078
_shelx_hkl_checksum              1817
_shelx_fab_checksum              37695