A homoleptic tris(diphosphacyclobutadiene) tripledecker sandwich complex
Rödl, Christian; Hierlmeier, Gabriele; Wolf, Robert; Chemical Communications  (2022) –; doi:10.1039/D2CC04601F

data_7130767
_publ_section_title
;
 A homoleptic tris(diphosphacyclobutadiene) tripledecker sandwich complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04601F
_journal_year                    2022
_chemical_formula_moiety         'C30 H54 Co2 P6'
_chemical_formula_sum            'C30 H54 Co2 P6'
_chemical_formula_weight         718.41
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-05 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.105(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9927(3)
_cell_length_b                   17.6107(5)
_cell_length_c                   10.2590(3)
_cell_measurement_reflns_used    10634
_cell_measurement_temperature    122.98(14)
_cell_measurement_theta_max      74.2580
_cell_measurement_theta_min      4.9680
_cell_volume                     1715.98(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.98(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  27.00   1.00    4.00    --  -44.08  38.00 150.00   77
  2  \w   -118.00  30.00   1.00    4.00    --  -44.08   0.00 120.00  148
  3  \w    -98.00  -3.00   1.00    4.00    --  -44.08 127.00-103.00   95
  4  \w      3.00  98.00   1.00    4.00    --   44.08-127.00-179.00   95
  5  \w     23.00 109.00   1.00   16.00    --  104.50 -94.00 -30.00   86
  6  \w     33.00 121.00   1.00   16.00    --  104.50-125.00 -90.00   88
  7  \w     36.00  98.00   1.00   16.00    --  104.50 -45.00 -60.00   62
  8  \w     68.00 178.00   1.00   16.00    --  104.50  15.00 -30.00  110
  9  \w     27.00 141.00   1.00   16.00    --  104.50 -15.00   0.00  114
 10  \w     36.00  98.00   1.00   16.00    --  104.50 -45.00  90.00   62
 11  \w     33.00 121.00   1.00   16.00    --  104.50-125.00 120.00   88
 12  \w     82.00 173.00   1.00   16.00    --  104.50  45.00   0.00   91
 13  \w     33.00 121.00   1.00   16.00    --  104.50-125.00 -30.00   88
 14  \w     32.00  91.00   1.00   16.00    --  104.50 -30.00-180.00   59
 15  \w     32.00  91.00   1.00   16.00    --  104.50 -30.00 -30.00   59
 16  \w     33.00 121.00   1.00   16.00    --  104.50-125.00  90.00   88
 17  \w     32.00  91.00   1.00   16.00    --  104.50 -30.00 120.00   59
 18  \w     35.00 130.00   1.00   16.00    --  104.50 -61.00-180.00   95
 19  \w     23.00 109.00   1.00   16.00    --  104.50 -94.00-180.00   86
 20  \w     23.00 109.00   1.00   16.00    --  104.50 -94.00 120.00   86
 21  \w   -113.00 -73.00   1.00    4.00    --  -44.08 -57.00  60.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1004287000
_diffrn_orient_matrix_UB_12      -0.0685804000
_diffrn_orient_matrix_UB_13      -0.0388495000
_diffrn_orient_matrix_UB_21      0.1273407000
_diffrn_orient_matrix_UB_22      -0.0540916000
_diffrn_orient_matrix_UB_23      0.0357077000
_diffrn_orient_matrix_UB_31      -0.0032706000
_diffrn_orient_matrix_UB_32      -0.0048059000
_diffrn_orient_matrix_UB_33      0.1489047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            21151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         74.542
_diffrn_reflns_theta_min         5.023
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.351
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0415P)^2^+1.1890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3250
_reflns_number_total             3481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04601f2.cif
_cod_data_source_block           mp
_cod_original_cell_volume        1715.98(9)
_cod_database_code               7130767
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C30 H54 Co2 P6 '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C6(H6A,H6B,H6C),
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C),
  C5(H5A,H5B,H5C)
;
_shelx_res_checksum              58276
_shelx_hkl_checksum              27
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.636
_oxdiff_exptl_absorpt_empirical_full_min 0.738