Inter- versus Intramolecular Structural Manipulation of a Dichromium(II) Pacman Complex through Pressure Variation.
Stevens, Charlotte J.; Prescimone, Alessandro; Tuna, Floriana; McInnes, Eric J. L.; Parsons, Simon; Morrison, Carole A.; Arnold, Polly L.; Love, Jason B.; Inorganic chemistry 55 (2016) 214–220; doi:10.1021/acs.inorgchem.5b02151

data_4346803
_publ_section_title
;
 Inter- versus Intramolecular Structural Manipulation of a Dichromium(II)
 Pacman Complex through Pressure Variation.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              214
_journal_page_last               220
_journal_paper_doi               10.1021/acs.inorgchem.5b02151
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        C.Stevens
_chemical_formula_moiety         'C48 H46 Cr2 N8'
_chemical_formula_sum            'C48 H46 Cr2 N8'
_chemical_formula_weight         838.94
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'from 0.86 GPa structure'
_audit_creation_date             2014-08-21
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 116.722(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5598(16)
_cell_length_b                   13.2590(15)
_cell_length_c                   15.0110(15)
_cell_measurement_reflns_used    3799
_cell_measurement_temperature    300
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_volume                     3655.0(6)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_pressure         1600000
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.646
_diffrn_measured_fraction_theta_max 0.646
_diffrn_measurement_device       'Rigaku Saturn 724 CCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type
'Synchrotron - Diamond Light Source Beamline I19'
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7894
_diffrn_reflns_theta_full        17.722
_diffrn_reflns_theta_max         17.722
_diffrn_reflns_theta_min         2.287
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method
; 
 
;
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0708
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         1823
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.0005935
_refine_ls_shift/su_mean         0.0000334
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.400 0.203 0.283 0.823E-01 0.177 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0603
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0451
_reflns_limit_h_max              22
_reflns_limit_h_min              -25
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1823
_reflns_number_total             2437
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0500
_oxford_refine_ls_scale          0.1293(3)
_oxford_reflns_number_all        2418
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'crpak3 in C2/c'
_cod_data_source_file            1_60GPa.cif
_cod_data_source_block           1_60GPa
_cod_original_cell_volume        3655.0(4)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4346803