Insertion reactions of β-diketiminate-stabilised calcium amides with 1,3-dialkylcarbodiimides
Barrett, Anthony G. M.; Crimmin, Mark R.; Hill, Michael S.; Hitchcock, Peter B.; Procopiou, Panayiotis A.; Dalton Transactions  (2008) 4474–4481; doi:10.1039/b717383k

data_7003601
_publ_section_title
;
 Insertion reactions of \b-diketiminate-stabilised calcium amides with
 1,3-dialkylcarbodiimides
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4474
_journal_page_last               4481
_journal_paper_doi               10.1039/b717383k
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H81 Ca N5 O'
_chemical_formula_sum            'C58 H81 Ca N5 O'
_chemical_formula_weight         904.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-10-20T12:34:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0903(3)
_cell_length_b                   19.8612(6)
_cell_length_c                   18.1455(6)
_cell_measurement_reflns_used    24833
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5273.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.264263E-1
_diffrn_orient_matrix_UB_12      0.130677E-1
_diffrn_orient_matrix_UB_13      -0.433953E-1
_diffrn_orient_matrix_UB_21      -0.629709E-1
_diffrn_orient_matrix_UB_22      0.3446E-2
_diffrn_orient_matrix_UB_23      -0.33887E-1
_diffrn_orient_matrix_UB_31      -0.26459E-2
_diffrn_orient_matrix_UB_32      0.485018E-1
_diffrn_orient_matrix_UB_33      0.140995E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.055
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32780
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         10342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+2.7982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                7206
_reflns_number_total             10342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717383k.txt
_cod_data_source_block           (7)-oct1206
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7003601