Mechanochemically directed metathesis in Group 2 chemistry: Calcium amide formation without solvent
Speight, Isaiah R.; Chmely, Stephen C.; Hanusa, Timothy P.; Rheingold, Arnold L.; Chemical Communications  (2019) –; doi:10.1039/C8CC10155H

data_7122892
_publ_section_title
;
 Mechanochemically directed metathesis in Group 2 chemistry: Calcium amide
 formation without solvent
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10155H
_journal_year                    2019
_chemical_formula_sum            'C18 H54 Ca K N3 Si6'
_chemical_formula_weight         560.36
_chemical_name_systematic
; 
 ? 
;
_chemical_properties_physical    Moisture-sensitive
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-12-04 deposited with the CCDC.
2019-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                93.148(5)
_cell_angle_beta                 91.419(2)
_cell_angle_gamma                111.817(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6477(8)
_cell_length_b                   11.2357(9)
_cell_length_c                   19.398(2)
_cell_measurement_reflns_used    9615
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.52
_cell_volume                     1745.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25442
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.358
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         7444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                6582
_reflns_number_total             7444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc10155h2.cif
_cod_data_source_block           vand70
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1745.0(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7122892