Synthesis of a "Super Bulky" Guanidinate Possessing an Expandable Coordination Pocket.
Maity, Arnab K.; Fortier, Skye; Griego, Leonel; Metta-Magaña, Alejandro J; Inorganic chemistry 53 (2014) 8155–; doi:10.1021/ic501219q

data_4340475
_publ_section_title
;
 Synthesis of a &quot;Super Bulky&quot; Guanidinate Possessing an
 Expandable Coordination Pocket.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8155
_journal_paper_doi               10.1021/ic501219q
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C36.5 H33 N)'
_chemical_formula_sum            'C73 H66 N2'
_chemical_formula_weight         971.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                69.174(2)
_cell_angle_beta                 80.489(2)
_cell_angle_gamma                76.285(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5162(10)
_cell_length_b                   13.9456(13)
_cell_length_c                   18.8607(17)
_cell_measurement_temperature    100(2)
_cell_volume                     2739.5(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27105
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.817
_diffrn_reflns_theta_min         1.160
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0564
_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^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6682
_reflns_number_total             10489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501219q_si_001.cif
_cod_data_source_block           Bulkycarbo
_cod_depositor_comments
'Adding full bibliography for 4340472--4340475.cif.'
_cod_database_code               4340475
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H43(0.022) H41(0.022) H60A(0.041) H60B(0.041) H60C(0.041)
 H59A(0.045) H59B(0.045) H59C(0.045) H61A(0.047) H61B(0.047) H61C(0.047)
 H45(0.024) H57(0.032) H49(0.04) H51(0.032) H47(0.031) H55(0.039) H53(0.033)
 H56(0.039) H54(0.038) H50(0.039) H48(0.039) H62(0.022) H64(0.028) H68(0.03)
 H67(0.036) H71(0.034) H65(0.035) H66(0.038) H70(0.03) H72(0.038) H73(0.037)
 H74(0.032) H6(0.023) H4(0.023) H25(0.024) H8(0.024) H27(0.032) H20(0.032)
 H10(0.031) H14(0.032) H12(0.042) H22A(0.046) H22B(0.046) H22C(0.046)
 H33(0.032) H35(0.04) H31(0.034) H37(0.034) H23A(0.049) H23B(0.049) H23C(0.049)
 H13(0.041) H24A(0.047) H24B(0.047) H24C(0.047) H18(0.043) H16(0.04) H36(0.041)
 H28(0.039) H19(0.038) H29(0.043) H30(0.04) H34(0.037) H11(0.039) H17(0.05)
 Fixed X: H43(0.7717) H41(0.8445) H60A(0.8452) H60B(0.9022) H60C(0.7718)
 H59A(1.0576) H59B(1.0795) H59C(1.0224) H61A(0.8336) H61B(0.9632) H61C(0.945)
 H45(0.6268) H57(0.6931) H49(0.8315) H51(0.5811) H47(0.9251) H55(0.9457)
 H53(0.8866) H56(0.7957) H54(0.9892) H50(0.6331) H48(0.9764) H62(0.5346)
 H64(0.4693) H68(0.7804) H67(0.796) H71(0.5954) H65(0.4853) H66(0.6523)
 H70(0.519) H72(0.794) H73(0.9142) H74(0.8366) C38(0.5) H6(0.2736) C1(0)
 H4(0.34) H25(0.0355) H8(0.1176) H27(-0.0475) H20(0.3581) H10(0.0585)
 H14(0.4112) H12(0.2888) H22A(0.5177) H22B(0.5859) H22C(0.5582) H33(0.0293)
 H35(0.312) H31(0.2676) H37(0.3409) H23A(0.2834) H23B(0.4138) H23C(0.3423)
 H13(0.4463) H24A(0.4628) H24B(0.4893) H24C(0.3582) H18(0.4402) H16(0.2075)
 H36(0.4257) H28(-0.063) H19(0.4605) H29(0.087) H30(0.2532) H34(0.1133)
 H11(0.0944) H17(0.31)
 Fixed Y: H43(0.307) H41(0.069) H60A(0.2105) H60B(0.3106) H60C(0.3193)
 H59A(0.1721) H59B(0.2225) H59C(0.1223) H61A(0.4048) H61B(0.3938) H61C(0.3499)
 H45(-0.0658) H57(-0.2603) H49(-0.1233) H51(-0.0422) H47(-0.1413) H55(-0.3633)
 H53(-0.0637) H56(-0.3937) H54(-0.1974) H50(-0.0671) H48(-0.1635) H62(0.2345)
 H64(0.4105) H68(0.3374) H67(0.5109) H71(0.1248) H65(0.5843) H66(0.6339)
 H70(0.2112) H72(0.0397) H73(0.0377) H74(0.1219) C38(0) H6(0.4425) C1(0.5)
 H4(0.2169) H25(0.6002) H8(0.325) H27(0.5651) H20(0.4389) H10(0.1658)
 H14(0.1614) H12(-0.107) H22A(0.1721) H22B(0.1737) H22C(0.2746) H33(0.7868)
 H35(0.8755) H31(0.6596) H37(0.5836) H23A(0.1734) H23B(0.1067) H23C(0.1149)
 H13(-0.0191) H24A(0.3666) H24B(0.2597) H24C(0.3253) H18(0.4683) H16(0.2883)
 H36(0.7112) H28(0.5943) H19(0.51) H29(0.6531) H30(0.6844) H34(0.9126) H11(-
 0.0141) H17(0.3598)
 Fixed Z: H43(0.3656) H41(0.2844) H60A(0.1663) H60B(0.1288) H60C(0.1696)
 H59A(0.2955) H59B(0.207) H59C(0.2415) H61A(0.2486) H61B(0.207) H61C(0.2961)
 H45(0.399) H57(0.4565) H49(0.1214) H51(0.2759) H47(0.3216) H55(0.6034)
 H53(0.4679) H56(0.5509) H54(0.5625) H50(0.1588) H48(0.2042) H62(0.4941)
 H64(0.4151) H68(0.5082) H67(0.4603) H71(0.7469) H65(0.3672) H66(0.3868)
 H70(0.6306) H72(0.7539) H73(0.6429) H74(0.5262) C38(0.5) H6(0.2342) C1(0)
 H4(0.1408) H25(0.1294) H8(0.0151) H27(0.2577) H20(-0.018) H10(0.0752)
 H14(0.0226) H12(0.1032) H22A(0.1869) H22B(0.2517) H22C(0.1809) H33(0.0621)
 H35(-0.0816) H31(0.2004) H37(0.0665) H23A(0.3352) H23B(0.3435) H23C(0.277)
 H13(0.0619) H24A(0.276) H24B(0.3421) H24C(0.3353) H18(-0.2385) H16(-0.1124)
 H36(-0.0299) H28(0.3721) H19(-0.1336) H29(0.4022) H30(0.3166) H34(-0.0355)
 H11(0.1084) H17(-0.2278)
;
_shelx_res_checksum              10531
_shelx_hkl_checksum              42782