The First Chelate-Free Crystal Structure of a Silicide Transition Metal Complex [K0.28Rb7.72Si9Ni(CO)2]2·16NH3
Gärtner, Stefanie; Hamberger, Markus; Korber, Nikolaus; Crystals 5 (2015) 275–; doi:10.3390/cryst5030275

data_1529351
_publ_section_title
;
 The First Chelate-Free Crystal Structure of a Silicide Transition Metal
 Complex [K0.28Rb7.72Si9Ni(CO)2]2&#x00B7;16NH3
;
_journal_issue                   3
_journal_name_full               Crystals
_journal_page_first              275
_journal_paper_doi               10.3390/cryst5030275
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety
'(K +), (Rb +), ([(Si9 Ni (CO)2)2] 8-), (H3 N)'
_chemical_formula_sum            'C4 H48 K0.28 N16 Ni2 O4 Rb7.72 Si18'
_chemical_formula_weight         1678.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.669(6)
_cell_length_b                   9.919(2)
_cell_length_c                   19.894(4)
_cell_measurement_temperature    123(2)
_cell_volume                     5680(2)
_computing_cell_refinement       'Stoe & Cie, 2002'
_computing_data_collection       'Stoe & Cie, 2002'
_computing_data_reduction        'Stoe & Cie, 2002'
_computing_molecular_graphics    'Brandenburg, 2012'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'Palatinus & Chapuis (2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46537
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.640
_diffrn_reflns_theta_min         2.318
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.676
_exptl_absorpt_correction_T_max  0.4480
_exptl_absorpt_correction_T_min  0.3638
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'analytical from crystal shape (Stoe & Cie, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_preparation
'Crystal mounting in liquid nitrogen cooled perflourether oil.'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6534
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             6534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s1.cif
_cod_data_source_block           '[K0.14Rb3.86Si9Ni(CO)2]2_16NH3'
_cod_database_code               1529351
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Rb4 \\sim K4A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001
3. Others
 Sof(K4A)=0.5*(1-FVAR(2))
 Sof(Rb4)=0.5*FVAR(2)
 Fixed Sof: Rb5(0.5)
 Fixed X: H2A(0.399281) H2B(0.392509) H2C(0.36713) H3A(0.426089) H3B(0.404579)
 H3C(0.4287) H8A(0.4257) H8B(0.37732) H8C(0.38905) H4A(0.57688) H4B(0.58014)
 H4C(0.54873) H1A(0.286029) H1B(0.28634) H1C(0.32659)
 Fixed Y: H2A(0.47518) H2B(0.36413) H2C(0.489419) H3A(0.70195) H3B(0.770469)
 H3C(0.84789) H8A(0.48796) H8B(0.447009) H8C(0.58791) H4A(1.107121)
 H4B(1.10977) H4C(1.20127) H1A(0.446949) H1B(0.397341) H1C(0.376749)
 Fixed Z: H2A(0.199281) H2B(0.14903) H2C(0.126301) H3A(0.24897) H3B(0.18095)
 H3C(0.245049) H8A(0.34777) H8B(0.326361) H8C(0.321941) H4A(0.245709)
 H4B(0.320331) H4C(0.26912) H1A(0.54752) H1B(0.47894) H1C(0.543241)
4.a Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C), N7(H7A,H7B,H7C), N6(H6A,H6B,H6C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'