Synthesis of heteroleptic calcium amide complexes <i>via</i> manipulation of the Schlenk equilibrium.
de Vere-Tucker, Matthew; Slawin, Alexandra M. Z.; Cordes, David B.; Stasch, Andreas; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1708–1715; doi:10.1039/d5dt02949j

data_7720446
_publ_section_title
;
 Synthesis of heteroleptic calcium amide complexes <i>via</i> manipulation
 of the Schlenk equilibrium.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1708
_journal_page_last               1715
_journal_paper_doi               10.1039/d5dt02949j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C66 H98 Ca N4, 0.5(C4 H10 O)'
_chemical_formula_sum            'C68 H103 Ca N4 O0.5'
_chemical_formula_weight         1024.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-06-04
_audit_creation_method           'by CrystalStructure 4.3'
_audit_update_record
;
2025-12-08 deposited with the CCDC.	2025-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.774(4)
_cell_angle_beta                 91.907(4)
_cell_angle_gamma                112.633(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7340(6)
_cell_length_b                   13.0655(7)
_cell_length_c                   20.7474(9)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    173
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      1.68
_cell_volume                     3183.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2019/3 (Sheldrick, 2015B)'
_computing_structure_solution    'SHELXT Version 2018/2 (Sheldrick, 2015A)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1731
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            82754
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         1.689
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1126.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.24
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     709
_refine_ls_number_reflns         9140
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.9962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5355
_reflns_number_total             9140
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d5dt02949j2.cif
_cod_data_source_block           7
_cod_database_code               7720446
_shelx_res_checksum              60683
_shelx_hkl_checksum              85217