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_7041816
_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         'C62 H92 Ca2 N4 O2, C6 H6'
_chemical_formula_sum            'C68 H98 Ca2 N4 O2'
_chemical_formula_weight         1083.66
_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             2016-07-18
_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                 100.888(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3510(5)
_cell_length_b                   16.3688(6)
_cell_length_c                   15.0996(5)
_cell_measurement_reflns_used    5165
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4680
_cell_measurement_theta_min      4.2810
_cell_volume                     3240.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -62.00  31.00   1.00    1.00    --  -41.69  38.00   0.00   93
  2  \w    -74.00  21.00   1.00    1.00    --  -41.69  19.00 -90.00   95
  3  \w    113.00 149.00   1.00    1.50    --  106.00  61.00-180.00   36
  4  \w    130.00 174.00   1.00    1.50    --  106.00  61.00-120.00   44
  5  \w     99.00 165.00   1.00    1.50    --  106.00 125.00   0.00   66
  6  \w     89.00 173.00   1.00    1.50    --  106.00  45.00 -90.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113151000
_diffrn_orient_matrix_UB_12      -0.0623625000
_diffrn_orient_matrix_UB_13      -0.0740635000
_diffrn_orient_matrix_UB_21      0.0924633000
_diffrn_orient_matrix_UB_22      -0.0381170000
_diffrn_orient_matrix_UB_23      0.0628447000
_diffrn_orient_matrix_UB_31      -0.0716509000
_diffrn_orient_matrix_UB_32      -0.0589106000
_diffrn_orient_matrix_UB_33      0.0371194000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11176
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         4.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.856
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
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    1.111
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.7101
_exptl_crystal_size_mid          0.2148
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0590P)^2^+0.9470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5429
_reflns_number_total             5890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04659b2.cif
_cod_data_source_block           hasj160715a
_cod_depositor_comments
'Adding full bibliography for 7041815--7041821.cif.'
_cod_database_code               7041816
_chemical_oxdiff_formula         'C H N Ca O '
_reflns_odcompleteness_completeness 78.54
_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:
 C15(H15), C12(H12), C24(H24), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C9(H9), C22(H22), C20(H20), C21(H21), C33(H33), C32(H32),
 C34(H34)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-15
_olex2_submission_original_sample_id hasj160715a
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.740
_oxdiff_exptl_absorpt_empirical_full_min 0.653