Introducing Stereogenic Centers to Group XIV Metallatranes.
Glowacki, Britta; Lutter, Michael; Alnasr, Hazem; Seymen, Rana; Hiller, Wolf; Jurkschat, Klaus; Inorganic chemistry  (2017) –; doi:10.1021/acs.inorgchem.6b03126

data_4345664
_publ_section_title
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 Introducing Stereogenic Centers to Group XIV Metallatranes.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b03126
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C22 H37 N O7 Sn, C7 H8'
_chemical_formula_sum            'C29 H45 N O7 Sn'
_chemical_formula_weight         638.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-29
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_cell_angle_alpha                90
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_cell_length_a                   7.0878(3)
_cell_length_b                   15.2637(13)
_cell_length_c                   27.1491(13)
_cell_measurement_reflns_used    3222
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.4750
_cell_measurement_theta_min      2.6050
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'XT (Sheldrick, 2015)'
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0560
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.879
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 0.879
_diffrn_reflns_Laue_measured_fraction_max 0.780
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            11725
_diffrn_reflns_point_group_measured_fraction_full 0.895
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.457
_diffrn_reflns_theta_min         2.617
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.009
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_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.810
_reflns_number_gt                5298
_reflns_number_total             6336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03126_si_002.cif
_cod_data_source_block           comp4
_cod_original_cell_volume        2937.1(3)
_cod_database_code               4345664
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01(4) -0.01(4)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C23(H23A,H23B), C33(H33A,H33B), C49(H49A,H49B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C2L(H2L), C3L(H3L), C4L(H4L), C5L(H5L), C6L(H6L)
3.c Idealised Me refined as rotating group:
 C7L(H7LA,H7LB,H7LC), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'