Chemically and electrochemically induced expansion and contraction of a ferrocene rotor
Scottwell, Synøve Ø.; Elliott, Anastasia B. S.; Shaffer, Karl J.; Nafady, Ayman; McAdam, C. John; Gordon, Keith C.; Crowley, James D.; Chemical Communications (Cambridge, United Kingdom) 51 (2015) 8161–8164; doi:10.1039/c5cc01973g

data_7117092
_publ_section_title
;
 Chemically and electrochemically induced expansion and contraction of a
 ferrocene rotor
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   38
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              8161
_journal_page_last               8164
_journal_paper_doi               10.1039/c5cc01973g
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C90 H78 Cl2 Cu2 Fe N8 O8'
_chemical_formula_weight         1653.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.0870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.1611(2)
_cell_length_b                   52.0625(9)
_cell_length_c                   20.5495(3)
_cell_measurement_reflns_used    60571
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.9960
_cell_measurement_theta_min      3.3730
_cell_volume                     18669.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3449
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            217551
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.5084
_exptl_absorpt_correction_T_min  0.3490
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6848
_exptl_crystal_size_max          0.4910
_exptl_crystal_size_mid          0.4185
_exptl_crystal_size_min          0.2881
_platon_squeeze_details
;
The packing of the crystal shows sizeable solvent channels containing significant 
amounts of diffuse electron density, accounted for by disordered solvent which 
could not be modelled as discrete molecules. This includes a minimum of 5 highly 
disordered acetonitrile molecules that could be located in the asymmetric unit, but 
were too disordered to refine. As such, PLATON SQUEEZE was employed to calculate 
the contribution to the diffraction from the solvent channels and thereby produced a 
set of solvent-free diffraction intensities. 

SQUEEZE estimated 8 voids with a total contribution of approximately 1276 electrons 
per unit cell. Due to this being a monoclinic space group with 4 asymmetric units per 
unit cell, this amounts to approximately 1276/4 = 319 electrons per asymmetric unit. 
This can be accounted for by 10 molecules of acetonitrile (10x22 = 220) and 10 
molecules of water (10x10 = 100) per asymmetric unit.
;
_refine_diff_density_max         3.286
_refine_diff_density_min         -1.694
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2023
_refine_ls_number_reflns         34176
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.1085
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1573P)^2^+47.0202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2930
_refine_ls_wR_factor_ref         0.3008
_reflns_number_gt                27795
_reflns_number_total             34176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01973g2.cif
_cod_data_source_block           c:\users\sscott\desktop\sos250~2\sos250
_cod_database_code               7117092