Triethylphosphine as a molecular gear — phase transitions in ferrocenyl‒acetylide‒gold(I)
Makal, Anna; Acta Crystallographica Section B 74 (2018) –; doi:10.1107/S2052520618010399

data_2108283
_publ_section_title
;
 Triethylphosphine as a molecular gear --- phase transitions in
 ferrocenyl--acetylide--gold(I)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520618010399
_journal_volume                  74
_journal_year                    2018
_chemical_formula_moiety         'C18 H24 Au Fe P'
_chemical_formula_sum            'C18 H24 Au Fe P'
_chemical_formula_weight         524.16
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P -2a -2ab'
_space_group_name_H-M_alt        'P b 21 a'
_symmetry_space_group_name_Hall  'P -2a -2ab'
_symmetry_space_group_name_H-M   'P b 21 a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.872(18)
_cell_length_b                   11.644(16)
_cell_length_c                   21.96(3)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    140.0(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.46
_cell_volume                     3547(8)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140.0(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker kappa APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23957
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.284
_diffrn_reflns_theta_min         0.927
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.160
_exptl_absorpt_correction_T_max  0.5521
_exptl_absorpt_correction_T_min  0.2852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.124
_refine_diff_density_max         8.546
_refine_diff_density_min         -6.757
_refine_diff_density_rms         0.391
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7862
_refine_ls_number_restraints     493
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0863
_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^)+(0.0001P)^2^+360.9662P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2137
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                7010
_reflns_number_total             7862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            um5013sup1.cif
_cod_data_source_block           1-140k
_cod_original_cell_volume        3548(8)
_cod_database_code               2108283
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.396
_shelx_estimated_absorpt_t_min   0.243
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(3)
 0.45(3)
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. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim Au2: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C12 \\sim C11 \\sim Au1: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
4. Rigid body (RIGU) restrains
 C5, Au1, P1, C12, C13, C15, C17, C11, C14, C16, C18, C1, Fe1, C2, C3, C4, C6,
 C7, C8, C9, C10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Au2, P2, C32, C33, C35, C37, C31, C34, C36, C38, C21, Fe2, C22, C25, C23, C24,
  C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Ternary CH refined with riding coordinates:
 C24(H24), C30(H30)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C33(H33A,H33B), C35(H35A,
 H35B), C37(H37A,H37B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_olex2_exptl_crystal_mounting_method 'Paratone N'
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108283