Synthesis and characterization of cyclodiphosphazanes embedded macrocycle tetrabromo-resorcin[4]arene-tetrakis(cyclodiphospha-zane) and its tetra-rhodium(I) complex
Pandey, Madhusudan Kumar; Sheokand, Sonu; Balakrishna, Maravanji Shivaramaiah; Dalton Transactions  (2023) –; doi:10.1039/D3DT00880K

data_7712753
_publ_section_title
;
 Synthesis and characterization of cyclodiphosphazanes embedded macrocycle
 tetrabromo-resorcin[4]arene-tetrakis(cyclodiphospha-zane) and its
 tetra-rhodium(I) complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00880K
_journal_year                    2023
_chemical_formula_moiety         '2(C108 H152 Br4 Cl4 N8 O8 P8 Rh4)'
_chemical_formula_sum            'C216 H304 Br8 Cl8 N16 O16 P16 Rh8'
_chemical_formula_weight         5622.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-23 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.9022(9)
_cell_length_b                   37.7479(10)
_cell_length_c                   12.5306(4)
_cell_measurement_reflns_used    26707
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.9180
_cell_measurement_theta_min      1.7860
_cell_volume                     15562.9(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1771
_diffrn_reflns_av_unetI/netI     0.1066
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            87929
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.821
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45534
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       plate
_exptl_crystal_F_000             5712
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.286
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.039(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         14156
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0719
_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^)+(0.0937P)^2^+28.7305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1877
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10699
_reflns_number_total             14156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00880k2.cif
_cod_data_source_block           compound-2
_cod_database_code               7712753
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.961(17)
 0.039(17)
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. Restrained distances
 C5-C6_$1 \\sim C5-C6A_$1
 with sigma of 0.02
 C6-C7_$2 \\sim C6A_$2-C7A_$3
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C5-C7 \\sim C5-C7A
 with sigma of 0.04
 C6-C8_$2 \\sim C6A_$2-C8A_$3
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C59) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C49) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C21) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Rh1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq,
Uanis(C7A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C37) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C36) = Uanis(C35) = Uanis(C4)
Uanis(C37) = Uanis(C36) = Uanis(C35) = Uanis(C4)
Uanis(C9A) = Uanis(C8A) = Uanis(C7A) = Uanis(C8) = Uanis(C9) = Uanis(C7) =
Uanis(C6)
5. Others
 Fixed Sof: H5A(0.55) H5B(0.45) C6(0.55) H6A(0.55) H6B(0.55) C7(0.55)
 H7A(0.55) H7B(0.55) C8(0.55) H8A(0.55) H8B(0.55) C9(0.55) C6A(0.45) H6AA(0.45)
 H6AB(0.45) C7A(0.45) H7AA(0.45) H7AB(0.45) C8A(0.45) H8AA(0.45) H8AB(0.45)
 C9A(0.45)
6.a Ternary CH refined with riding coordinates:
 C5(H5A), C5(H5B), C22(H22), C25(H25), C34(H34), C26(H26), C29(H29), C56(H56),
 C52(H52), C55(H55), C51(H51)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C23(H23A,H23B), C24(H24A,H24B), C57(H57A,
 H57B), C53(H53A,H53B), C58(H58A,H58B), C54(H54A,H54B), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8A,H8B), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C4(H4A,H4B),
  C35(H35A,H35B), C36(H36A,H36B)
6.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C10(H10), C59(H59), C33(H33)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C48(H48A,H48B,H48C), C20(H20A,H20B,H20C), C19(H19A,
 H19B,H19C), C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              33749
_shelx_fab_checksum              44081
_olex2_submission_special_instructions 'No special instructions were received'