Accurate crystal structures and chemical properties from NoSpherA2.
Kleemiss, Florian; Dolomanov, Oleg V.; Bodensteiner, Michael; Peyerimhoff, Norbert; Midgley, Laura; Bourhis, Luc J.; Genoni, Alessandro; Malaspina, Lorraine A.; Jayatilaka, Dylan; Spencer, John L.; White, Fraser; Grundkötter-Stock, Bernhard; Steinhauer, Simon; Lentz, Dieter; Puschmann, Horst; Grabowsky, Simon; Chemical science 12 (2020) 1675–1692; doi:10.1039/d0sc05526c

data_1559798
_publ_section_title
;
 Accurate crystal structures and chemical properties from NoSpherA2.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1675
_journal_page_last               1692
_journal_paper_doi               10.1039/d0sc05526c
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C24 H44 Os P2'
_chemical_formula_sum            'C24 H44 Os P2'
_chemical_formula_weight         584.789
_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_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-12
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.03.04 svn.rc2590c38 for OlexSys, GUI svn.r6014)
;
_audit_update_record
;
2020-09-28 deposited with the CCDC.	2020-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.563(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8918(1)
_cell_length_b                   13.7619(1)
_cell_length_c                   17.0714(2)
_cell_measurement_reflns_used    63613
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      36.3840
_cell_measurement_theta_min      3.5970
_cell_volume                     2530.34(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9986
_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     50.00 105.00   1.00    3.65    --   36.08 159.00  95.00   55
  2  \w      9.00 104.00   1.00    3.65    --   36.08  77.00   0.00   95
  3  \w     19.00 103.00   1.00    3.65    --   36.08  57.00-180.00   84
  4  \w     35.00 108.00   1.00    3.65    --   36.08 178.00 150.00   73
  5  \w     35.00 108.00   1.00    3.65    --   36.08 178.00  30.00   73
  6  \w      9.00 104.00   1.00    3.65    --   36.08  77.00  60.00   95
  7  \w    -33.00 105.00   1.00    3.65    --   36.08   0.00-180.00  138
  8  \w    -33.00 105.00   1.00    3.65    --   36.08   0.00  60.00  138
  9  \w     -4.00  86.00   1.00    3.65    --   36.08-118.00-143.00   90
 10  \w     35.00 108.00   1.00    3.65    --   36.08 178.00-150.00   73
 11  \w      9.00 104.00   1.00    3.65    --   36.08  77.00-180.00   95
 12  \w      9.00 104.00   1.00    3.65    --   36.08  77.00 -90.00   95
 13  \w      9.00 104.00   1.00    3.65    --   36.08  77.00 120.00   95
 14  \w     19.00 103.00   1.00    3.65    --   36.08  57.00 -90.00   84
 15  \w    -99.00 -11.00   1.00    3.65    --  -30.00 -38.00 -30.00   88
 16  \w    -99.00 -11.00   1.00    3.65    --  -30.00 -38.00 150.00   88
 17  \w    -31.00  63.00   1.00    3.65    --   36.08 -77.00  60.00   94
 18  \w      9.00 104.00   1.00    3.65    --   36.08  77.00 -30.00   95
 19  \w     35.00 108.00   1.00    3.65    --   36.08 178.00 -30.00   73
 20  \w     20.00 109.00   1.00    3.65    --   36.08-159.00  63.00   89
 21  \w    -98.00  -3.00   1.00    3.65    --  -30.00 -77.00 150.00   95
 22  \w    -98.00  -3.00   1.00    3.65    --  -30.00 -77.00  30.00   95
 23  \w    -97.00 -13.00   1.00    3.65    --  -30.00 -57.00-150.00   84
 24  \w    -49.00  39.00   1.00    3.65    --  -30.00  38.00-120.00   88
 25  \w    -97.00 -19.00   1.00    3.65    --  -30.00 -57.00  30.00   78
 26  \w      9.00 104.00   1.00    3.65    --   36.08  77.00-150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0251251000
_diffrn_orient_matrix_UB_12      0.0472240000
_diffrn_orient_matrix_UB_13      0.0076280000
_diffrn_orient_matrix_UB_21      -0.0031394000
_diffrn_orient_matrix_UB_22      -0.0060278000
_diffrn_orient_matrix_UB_23      0.0409225000
_diffrn_orient_matrix_UB_31      0.0607998000
_diffrn_orient_matrix_UB_32      -0.0198267000
_diffrn_orient_matrix_UB_33      0.0057471000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.9976
_diffrn_reflns_Laue_measured_fraction_max 0.9986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            196209
_diffrn_reflns_point_group_measured_fraction_full 0.9976
_diffrn_reflns_point_group_measured_fraction_max 0.9986
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.51
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7c (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.5047
_refine_diff_density_min         -0.5003
_refine_diff_density_rms         0.0793
_refine_ls_d_res_high            0.7000
_refine_ls_d_res_low             5.7986
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0722
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7723
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0717
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0119
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0005P)^2^+0.2531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0185
_refine_ls_wR_factor_ref         0.0189
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -15
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -11
_reflns_number_gt                7199
_reflns_number_total             7723
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0sc05526c2.cif
_cod_data_source_block           Os_PBE
_cod_depositor_comments
;Adding full bibliography for 1559792--1559798.cif.

 Adding full bibliography for 1559792--1559798.cif.
;
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1559798
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 H8, Os
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H7, Os
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_submission_special_instructions 'No special instructions were received'