Alkali metal complexes based on bisheterocyclomethanide ligands.
Kretsch, Johannes; Kreyenschmidt, Anne; Herbst-Irmer, Regine; Stalke, Dietmar; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12606–12612; doi:10.1039/c8dt01678j

data_7046644
_publ_section_title
;
 Alkali metal complexes based on bisheterocyclomethanide ligands.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12606
_journal_page_last               12612
_journal_paper_doi               10.1039/c8dt01678j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C27 H33 K N2 O8'
_chemical_formula_sum            'C27 H33 K N2 O8'
_chemical_formula_weight         552.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-04-26 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.913(3)
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_cell_length_c                   15.309(3)
_cell_measurement_reflns_used    8786
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4015
_cell_measurement_theta_min      2.2535
_cell_volume                     2675.1(9)
_computing_cell_refinement       'SAINT V8.38A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.38A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
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_computing_structure_solution
'SHELXT(G.M.Sheldrick,Acta Cryst.(2015)A71,3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33321
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.427
_diffrn_reflns_theta_min         1.855
_diffrn_source                   'BRUKER Rotating Anode'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2060 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5489
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.2234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4843
_reflns_number_total             5489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01678j2.cif
_cod_data_source_block           sad_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7046642--7046644.cif.'
_cod_database_code               7046644
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              26578