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_7041815
_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         'C32 H48 Ca N3'
_chemical_formula_sum            'C32 H48 Ca N3'
_chemical_formula_weight         514.81
_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     direct
_audit_creation_date             2016-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5639(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.88056(13)
_cell_length_b                   15.1230(2)
_cell_length_c                   22.2473(3)
_cell_measurement_reflns_used    5758
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.5860
_cell_measurement_theta_min      4.9240
_cell_volume                     2968.24(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      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega  -66.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000 -150.0000 92

  2 omega -110.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000    0.0000 94

  3 omega   82.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  -60.0000 69

  4 omega   95.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -180.0000 27

  5 omega   41.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -180.0000 49

  6 omega   40.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000    0.0000 75

  7 omega   36.00  128.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   90.0000 92

  8 omega   33.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   60.0000 76
;
_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      0.0757412000
_diffrn_orient_matrix_UB_12      0.0598427000
_diffrn_orient_matrix_UB_13      0.0507385000
_diffrn_orient_matrix_UB_21      -0.0893430000
_diffrn_orient_matrix_UB_22      0.0799659000
_diffrn_orient_matrix_UB_23      -0.0283787000
_diffrn_orient_matrix_UB_31      -0.1295763000
_diffrn_orient_matrix_UB_32      -0.0200266000
_diffrn_orient_matrix_UB_33      0.0384334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10589
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.695
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.985
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.893
_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    1.152
_exptl_crystal_description       needle
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.4586
_exptl_crystal_size_mid          0.0636
_exptl_crystal_size_min          0.0489
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0400P)^2^+0.8280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5198
_reflns_number_total             5747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04659b2.cif
_cod_data_source_block           hasj160613a
_cod_depositor_comments
'Adding full bibliography for 7041815--7041821.cif.'
_cod_original_cell_volume        2968.24(8)
_cod_database_code               7041815
_chemical_oxdiff_formula         'C H N Ca O Si'
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid body (RIGU) restrains
 C32, C31, N3, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: N3(0.5) C31(0.5) H31A(0.5) H31B(0.5) C35(0.5) H35A(0.5) H35B(0.5)
 N4(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C27(H27), C24(H24), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C35(H35A,H35B), C33(H33A,H33B), C34(H34A,H34B), C30(H30A,
 H30B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C22(H22), C20(H20), C10(H10), C9(H9), C21(H21)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C16(H16A,H16B,H16C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-13
_olex2_submission_special_instructions 'No special instructions were received'