Dimethylcalcium.
Wolf, Benjamin M.; Stuhl, Christoph; Maichle-Mössmer, Cäcilia; Anwander, Reiner; Journal of the American Chemical Society 140 (2018) 2373–2383; doi:10.1021/jacs.7b12984

data_4131919
_publ_section_title
;
 Dimethylcalcium.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2373
_journal_page_last               2383
_journal_paper_doi               10.1021/jacs.7b12984
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C52.5 H105.5 Ca2 O5'
_chemical_formula_weight         897.02
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.0270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0501(7)
_cell_length_b                   19.3522(10)
_cell_length_c                   22.1731(11)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.592
_cell_volume                     5596.3(5)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX3 v2016.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'XT, VERSION 2014/5,SHELXS-13 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            101158
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.397
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       block
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.202
_refine_diff_density_max         1.675
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         12349
_refine_ls_number_restraints     895
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0865P)^2^+7.9358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9835
_reflns_number_total             12349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b12984_si_002.cif
_cod_data_source_block           7_mo_BW379_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C52.50 H105.50 Ca2 O5'
_cod_database_code               4131919
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              44511
_shelx_hkl_checksum              3829