β-Diketiminate calcium hydride complexes: the importance of solvent effects.
Causero, Andrea; Ballmann, Gerd; Pahl, Jürgen; Färber, Christian; Intemann, Julia; Harder, Sjoerd; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1822–1831; doi:10.1039/c6dt04659b

data_7041819
_publ_section_title
;
 \b-Diketiminate calcium hydride complexes: the importance of solvent
 effects.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1822
_journal_page_last               1831
_journal_paper_doi               10.1039/c6dt04659b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C68 H106 Ca2 N6 O2'
_chemical_formula_sum            'C68 H106 Ca2 N6 O2'
_chemical_formula_weight         1119.74
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4825(2)
_cell_length_b                   13.02210(10)
_cell_length_c                   18.2443(2)
_cell_measurement_reflns_used    17845
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4220
_cell_measurement_theta_min      3.5420
_cell_volume                     3385.44(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  -90.0000 97

  2 omega  -68.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000   60.0000 96

  3 omega  -64.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -150.0000 95

  4 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000 -120.0000 74

  5 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000    0.0000 99

  6 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -90.0000 99

  7 omega   94.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000   30.0000 84

  8 omega   25.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -30.0000 84

  9 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -180.0000 99

 10 omega   34.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  -90.0000 87

 11 omega   31.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 99

 12 omega   25.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   30.0000 84

 13 omega   32.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000   60.0000 105

 14 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  150.0000 97

 15 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000    0.0000 97

 16 omega -116.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000 -120.0000 106

 17 omega -116.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000   90.0000 106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0721071000
_diffrn_orient_matrix_UB_12      0.0224118000
_diffrn_orient_matrix_UB_13      0.0506540000
_diffrn_orient_matrix_UB_21      0.0107831000
_diffrn_orient_matrix_UB_22      -0.1107073000
_diffrn_orient_matrix_UB_23      0.0300683000
_diffrn_orient_matrix_UB_31      0.0798301000
_diffrn_orient_matrix_UB_32      0.0351076000
_diffrn_orient_matrix_UB_33      0.0624251000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.100
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.3828
_exptl_crystal_size_mid          0.3238
_exptl_crystal_size_min          0.1131
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0640P)^2^+0.9850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5756
_reflns_number_total             6166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04659b2.cif
_cod_data_source_block           hasj161012a
_cod_depositor_comments
'Adding full bibliography for 7041815--7041821.cif.'
_cod_database_code               7041819
_chemical_oxdiff_formula         'C H N Ca O Si '
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24), C15(H15), C12(H12), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C9(H9), C22(H22), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C),
 C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C34(H34A,H34B,
 H34C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-10-12
_olex2_submission_original_sample_id hasj161012a
_olex2_submission_special_instructions 'No special instructions were received'