A Hydrogen Polyphosphide Salt of the First Homoleptic Strontium Ammine Complex: Synthesis and Structure Analysis of [Sr(NH~3~)~8~]HP~11~.NH~3~
Nikolaus Korber; Jörg Daniels; Inorganic Chemistry 36 (1997) 4906–4908; doi:10.1021/ic970664i

data_4323632
_publ_contact_author
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Dr. Nikolaus Korber
Institut f. Anorganische Chemie, Universit\"at Bonn
Gerhard-Domagk-Str. 1
D-53121 Bonn
Germany
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_publ_contact_author_email       korber@plumbum.chemie.uni-bonn.de
_publ_contact_author_fax         '228 73 5660'
_publ_contact_author_phone       '228 73 3591'
_publ_section_title
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 A Hydrogen Polyphosphide Salt of the First Homoleptic Strontium Ammine
 Complex: Synthesis and Structure Analysis of [Sr(NH~3~)~8~]HP~11~.NH~3~
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4906
_journal_page_last               4908
_journal_paper_doi               10.1021/ic970664i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         '(H24 N8 Sr 2+),(H P11 2-),(H3 N)'
_chemical_formula_sum            'H28 N9 P11 Sr'
_chemical_formula_weight         582.60
_chemical_name_systematic
;
strontium hydrogenundecaphosphide-ammonia(1/9)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.824(5)
_cell_length_b                   13.604(2)
_cell_length_c                   9.657(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2473.0(9)
_computing_cell_refinement       'CELDIM (CAD4 software)'
_computing_data_collection       'CAD4 software Version 5.0'
_computing_data_reduction        'MoLEN (ENRAF-NONIUS software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       'variable scan speed \w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5396
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.896
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(15)
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_hydrogen_treatment
;
noref except for refall for H1, HN9A, HN9B, HN9C
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2815
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.056
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_obs          0.0520
_refine_ls_shift/esd_max         -2.049
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+10.0110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1503
_refine_ls_wR_factor_obs         0.1293
_reflns_number_observed          2392
_reflns_number_total             2849
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970664i.cif
_cod_data_source_block           IC9706641
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+10.0110P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+10.0110P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323632