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_7041817
_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         'C66 H104 Ca2 N4 O2'
_chemical_formula_sum            'C66 H104 Ca2 N4 O2'
_chemical_formula_weight         1065.69
_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             2016-08-01
_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                 97.5028(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.98073(15)
_cell_length_b                   15.11446(17)
_cell_length_c                   18.0466(2)
_cell_measurement_reflns_used    7112
_cell_measurement_temperature    291.81(10)
_cell_measurement_theta_max      73.5630
_cell_measurement_theta_min      3.8180
_cell_volume                     3239.94(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_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      air
_diffrn_ambient_temperature      291.81(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  -90.0000 81

  2 omega  -79.00   37.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   19.0000 -150.0000 116

  3 omega  -94.00  -56.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000 -180.0000 38

  4 omega   39.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  -90.0000 59

  5 omega   50.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 41

  6 omega   38.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -150.0000 60

  7 omega   31.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   60.0000 60

  8 omega   52.00   89.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  150.0000 37

  9 omega   43.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  120.0000 55

 10 omega   25.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -95.0000  100.0000 69
;
_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      -0.0467746000
_diffrn_orient_matrix_UB_12      0.0234316000
_diffrn_orient_matrix_UB_13      0.0730994000
_diffrn_orient_matrix_UB_21      -0.1169063000
_diffrn_orient_matrix_UB_22      -0.0343142000
_diffrn_orient_matrix_UB_23      -0.0334503000
_diffrn_orient_matrix_UB_31      0.0312056000
_diffrn_orient_matrix_UB_32      -0.0930742000
_diffrn_orient_matrix_UB_33      0.0307768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11551
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         3.828
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.2716
_exptl_crystal_size_mid          0.1884
_exptl_crystal_size_min          0.1097
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0660P)^2^+1.0980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5302
_reflns_number_total             5888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04659b2.cif
_cod_data_source_block           hasj150130c
_cod_depositor_comments
'Adding full bibliography for 7041815--7041821.cif.'
_cod_original_cell_volume        3239.93(7)
_cod_database_code               7041817
_chemical_oxdiff_formula         'Ca N H C'
_reflns_odcompleteness_completeness 99.60
_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.a Ternary CH refined with riding coordinates:
 C27(H27), C12(H12), C15(H15), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C10(H10), C21(H21), C8(H8), C9(H9), C20(H20)
2.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C28(H28A,H28B,H28C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C13(H13A,H13B,
 H13C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-01-30
_olex2_submission_special_instructions 'No special instructions were received'