Synthetic and Structural Studies on Linear and Macrocyclic Pd- and Pt-Bridged Butterfly Fe/S Cluster Complexes
Song, Li-Cheng; Zhang, Long-Duo; Liu, Bei-Bei; Ding, Shu-Da; Chen, Hao; Xu, Xiu-Fang; Fan, Gui-Lan; Organometallics 36 (2017) 1419–; doi:10.1021/acs.organomet.7b00117

data_4089263
_publ_section_title
;
 Synthetic and Structural Studies on Linear and Macrocyclic Pd- and
 Pt-Bridged Butterfly Fe/S Cluster Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1419
_journal_paper_doi               10.1021/acs.organomet.7b00117
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C54 H38 Fe4 O12 P2 Pt S6'
_chemical_formula_sum            'C54 H38 Fe4 O12 P2 Pt S6'
_chemical_formula_weight         1551.63
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.993(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.633(4)
_cell_length_b                   23.032(5)
_cell_length_c                   22.401(5)
_cell_measurement_reflns_used    25986
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.7
_cell_volume                     7139(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
	Number of images: 90
	           Slice: -110.0000 - 70.0000
	     Image width: 2.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 44.9900
	          2theta: -20.0264
scan:
	Number of images: 70
	           Slice: -110.0000 - 30.0000
	     Image width: 2.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 44.9900
	          2theta: -20.0264
scan:
	Number of images: 60
	           Slice: -110.0000 - 10.0000
	     Image width: 2.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9900
	          2theta: -20.0264
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.067152
_diffrn_orient_matrix_UB_12      0.005235
_diffrn_orient_matrix_UB_13      -0.026209
_diffrn_orient_matrix_UB_21      -0.001546
_diffrn_orient_matrix_UB_22      0.041619
_diffrn_orient_matrix_UB_23      0.012273
_diffrn_orient_matrix_UB_31      0.002156
_diffrn_orient_matrix_UB_32      0.013414
_diffrn_orient_matrix_UB_33      -0.045214
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59960
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.717
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.015
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.763
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.105
_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     701
_refine_ls_number_reflns         12579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.5629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11047
_reflns_number_total             12579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00117_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089263
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.531
_olex2_refinement_description
;
1. 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
2.a Riding coordinates:
 C54(H54A,H54B,H54C)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C36(H36),
  C37(H37), C38(H38), C39(H39), C40(H40), C44(H44), C45(H45), C46(H46),
 C42(H42), C43(H43), C49(H49), C50(H50), C52(H52), C53(H53)
2.d Fitted hexagon refined as free rotating group:
 C44(C45,C46,C41,C42,C43)
2.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              45708
_shelx_hkl_checksum              40222
_shelx_fab_checksum              75207
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'