Two alternative approaches to access mixed hydride-amido zinc complexes: synthetic, structural and solution implications.
Roberts, Andrew J.; Clegg, William; Kennedy, Alan R.; Probert, Michael R.; Robertson, Stuart D.; Hevia, Eva; Dalton transactions (Cambridge, England : 2003) 44 (2015) 8169–8177; doi:10.1039/c5dt00312a

data_7034643
_publ_section_title
;
 Two alternative approaches to access mixed hydride-amido zinc complexes:
 synthetic, structural and solution implications.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8169
_journal_page_last               8177
_journal_paper_doi               10.1039/c5dt00312a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C66 H114 N6 Si4 Zn4,C4 H8 O'
_chemical_formula_sum            'C70 H122 N6 O Si4 Zn4'
_chemical_formula_weight         1437.57
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_audit_update_record
;
2015-01-06 deposited with the CCDC.
2015-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.153(7)
_cell_length_b                   16.412(5)
_cell_length_c                   22.139(7)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      2.33
_cell_volume                     8049(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Rigaku Saturn 724+ on kappa diffractometer'
_diffrn_measurement_method       'wide-frame \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53956
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.511
_diffrn_reflns_theta_min         1.497
_diffrn_source                   'Diamond beamline I19'
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.740
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 5006 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         15103
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0629
_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^)+(0.1180P)^2^+0.2877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1767
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                12203
_reflns_number_total             15103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00312a2.cif
_cod_data_source_block           eh15
_cod_depositor_comments
'Adding full bibliography for 7034643--7034645.cif.'
_cod_database_code               7034643
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2014-3